# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2205502'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-05
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 F N O6 Re'
_chemical_formula_sum            'C9 H5 F N O6 Re'
_chemical_formula_weight         428.34
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1094(2)
_cell_length_b                   8.1861(3)
_cell_length_c                   9.3662(3)
_cell_angle_alpha                92.147(3)
_cell_angle_beta                 94.856(2)
_cell_angle_gamma                90.442(3)
_cell_volume                     542.73(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8813
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3920
_cell_measurement_theta_min      4.7000
_shelx_estimated_absorpt_T_max   0.304
_shelx_estimated_absorpt_T_min   0.108
_exptl_absorpt_coefficient_mu    22.298
_exptl_absorpt_correction_T_max  0.385
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -4 0.0369
0 0 4 0.0369
3 0 0 0.0882
-3 1 1 0.0691
0 3 -1 0.0303
0 -3 1 0.0482
0 -2 3 0.0359
0 0 -5 0.0316

_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07

_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8892
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.461
_diffrn_reflns_theta_min         4.742
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  28.00   1.00    1.00    --  -42.61  57.00-180.00   97
  2  ω   -113.00 -16.00   1.00    1.00    --  -42.61 -57.00  30.00   97
  3  ω    -21.00  74.00   1.00    1.00    --   42.61 -77.00 -90.00   95
  4  ω     27.00  98.00   1.00    1.00    --   42.61-125.00-180.00   71
  5  ω    104.00 178.00   1.00    2.00    --  111.00 111.00  90.00   74
  6  ω     36.00 109.00   1.00    2.00    --  111.00-111.00  90.00   73
  7  ω     81.00 178.00   1.00    2.00    --  111.00  70.00 -79.10   97
  8  ω     36.00 135.00   1.00    2.00    --  111.00 -30.00 150.00   99
  9  ω    103.00 178.00   1.00    2.00    --  111.00  77.00 150.00   75
 10  ω     30.00 107.00   1.00    2.00    --  111.00 -94.00-150.00   77
 11  ω     37.00 142.00   1.00    2.00    --  111.00 -77.00-120.00  105
 12  ω     31.00 156.00   1.00    2.00    --  111.00 -15.00 -30.00  125
 13  ω     41.00 139.00   1.00    2.00    --  111.00 -61.00  60.00   98
 14  ω     36.00 109.00   1.00    2.00    --  111.00-111.00  30.00   73
 15  ω     36.00 109.00   1.00    2.00    --  111.00-111.00-150.00   73
 16  ω     36.00 109.00   1.00    2.00    --  111.00-111.00-180.00   73
 17  ω     87.00 178.00   1.00    2.00    --  111.00  30.00  30.00   91
 18  ω   -113.00 -16.00   1.00    1.00    --  -42.61 -57.00 -90.00   97
 19  ω     16.00 113.00   1.00    1.00    --   42.61  57.00-150.00   97
 20  ω     20.00 116.00   1.00    1.00    --   42.61  37.00 150.00   96
 21  ω     11.00  42.00   1.00    1.00    --   42.61  79.00  50.32   31
 22  ω     83.00 178.00   1.00    2.00    --  111.00  61.00-150.00   95
 23  ω     83.00 178.00   1.00    2.00    --  111.00  61.00-180.00   95
 24  ω     87.00 178.00   1.00    2.00    --  111.00  45.00 -30.00   91
 25  ω     84.00 178.00   1.00    2.00    --  111.00  57.00  90.44   94
 26  ω     66.00 178.00   1.00    2.00    --  111.00  15.00 120.00  112
 27  ω     84.00 178.00   1.00    2.00    --  111.00  59.00  21.93   94
 28  ω     87.00 178.00   1.00    2.00    --  111.00  45.00 150.00   91
 29  ω     83.00 178.00   1.00    2.00    --  111.00  61.00  60.00   95
 30  ω     83.00 178.00   1.00    2.00    --  111.00  61.00 -90.00   95
 31  ω     83.00 108.00   1.00    2.00    --  111.00  61.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1203131000
_diffrn_orient_matrix_UB_12      -0.0603932000
_diffrn_orient_matrix_UB_13      0.1171641000
_diffrn_orient_matrix_UB_21      -0.1795653000
_diffrn_orient_matrix_UB_22      0.0140727000
_diffrn_orient_matrix_UB_23      -0.1028500000
_diffrn_orient_matrix_UB_31      0.0241308000
_diffrn_orient_matrix_UB_32      -0.1778348000
_diffrn_orient_matrix_UB_33      -0.0546214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2189
_reflns_number_total             2196

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00482(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0145
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²+0.8041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0358
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.0931(4) 0.5820(4) 0.7281(3) 0.0196(6) Uani 1 1 d . . . . .
C2 C -0.0081(4) 0.2757(4) 0.6364(3) 0.0206(6) Uani 1 1 d . . . . .
C3 C 0.2860(4) 0.4135(4) 0.5353(3) 0.0209(6) Uani 1 1 d . . . . .
C4 C 0.3344(4) 0.0045(4) 0.7020(4) 0.0266(6) Uani 1 1 d . . . . .
H4 H 0.213668 -0.011051 0.651381 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4486(5) -0.1299(4) 0.7245(4) 0.0315(7) Uani 1 1 d . . . . .
H5 H 0.406672 -0.235623 0.689690 0.038 Uiso 1 1 calc R U . . .
C6 C 0.6228(5) -0.1086(4) 0.7977(4) 0.0288(7) Uani 1 1 d . . . . .
H6 H 0.703930 -0.198617 0.815432 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6767(4) 0.0482(4) 0.8449(3) 0.0247(6) Uani 1 1 d . . . . .
C8 C 0.5605(4) 0.1799(3) 0.8207(3) 0.0179(5) Uani 1 1 d . . . . .
C9 C 0.6075(4) 0.3562(3) 0.8635(3) 0.0166(5) Uani 1 1 d . . . . .
F1 F 0.8481(3) 0.0704(3) 0.9152(3) 0.0400(5) Uani 1 1 d . . . . .
N1 N 0.3878(3) 0.1555(3) 0.7491(3) 0.0177(5) Uani 1 1 d . . . . .
O1 O 0.0230(3) 0.7083(3) 0.7341(3) 0.0286(5) Uani 1 1 d . . . . .
O2 O -0.1424(3) 0.2119(3) 0.5831(2) 0.0292(5) Uani 1 1 d . . . . .
O3 O 0.3225(3) 0.4348(3) 0.4206(2) 0.0291(5) Uani 1 1 d . . . . .
O4 O 0.1571(3) 0.3246(3) 0.9438(2) 0.0188(4) Uani 1 1 d . . . . .
H4A H 0.185(7) 0.406(6) 1.001(5) 0.041(12) Uiso 1 1 d . . . . .
H4B H 0.048(7) 0.318(6) 0.939(5) 0.035(12) Uiso 1 1 d . . . . .
O5 O 0.7667(3) 0.3919(3) 0.9219(2) 0.0225(4) Uani 1 1 d . . . . .
O6 O 0.4776(3) 0.4579(2) 0.8358(2) 0.0181(4) Uani 1 1 d . . . . .
Re1 Re 0.21809(2) 0.37491(2) 0.72380(2) 0.01457(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
C1 O1 1.153(4) . ?
C1 Re1 1.921(3) . ?
C2 O2 1.151(4) . ?
C2 Re1 1.904(3) . ?
C3 O3 1.145(4) . ?
C3 Re1 1.907(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(5) . ?
C4 N1 1.338(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.371(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(5) . ?
C7 C8 1.377(4) . ?
C7 F1 1.342(3) . ?
C8 C9 1.510(4) . ?
C8 N1 1.358(4) . ?
C9 O5 1.243(3) . ?
C9 O6 1.265(4) . ?
N1 Re1 2.181(2) . ?
O4 H4A 0.85(5) . ?
O4 H4B 0.77(5) . ?
O4 Re1 2.194(2) . ?
O6 Re1 2.1370(19) . ?

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
O1 C1 Re1 177.6(3) . . ?
O2 C2 Re1 178.2(3) . . ?
O3 C3 Re1 178.2(3) . . ?
C5 C4 H4 118.8 . . ?
N1 C4 H4 118.8 . . ?
N1 C4 C5 122.4(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 H6 121.1 . . ?
C5 C6 C7 117.8(3) . . ?
C7 C6 H6 121.1 . . ?
C8 C7 C6 121.8(3) . . ?
F1 C7 C6 118.2(3) . . ?
F1 C7 C8 120.0(3) . . ?
C7 C8 C9 126.1(3) . . ?
N1 C8 C7 119.3(3) . . ?
N1 C8 C9 114.6(2) . . ?
O5 C9 C8 119.3(3) . . ?
O5 C9 O6 124.7(3) . . ?
O6 C9 C8 116.0(2) . . ?
C4 N1 C8 119.5(3) . . ?
C4 N1 Re1 125.6(2) . . ?
C8 N1 Re1 114.89(18) . . ?
H4A O4 H4B 105(5) . . ?
Re1 O4 H4A 112(3) . . ?
Re1 O4 H4B 103(3) . . ?
C9 O6 Re1 119.22(18) . . ?
C1 Re1 N1 170.79(10) . . ?
C1 Re1 O4 92.73(10) . . ?
C1 Re1 O6 96.44(10) . . ?
C2 Re1 C1 89.51(12) . . ?
C2 Re1 C3 87.34(12) . . ?
C2 Re1 N1 98.61(11) . . ?
C2 Re1 O4 94.96(10) . . ?
C2 Re1 O6 172.69(10) . . ?
C3 Re1 C1 89.87(13) . . ?
C3 Re1 N1 94.83(11) . . ?
C3 Re1 O4 176.54(10) . . ?
C3 Re1 O6 96.90(10) . . ?
N1 Re1 O4 82.28(8) . . ?
O6 Re1 N1 75.16(8) . . ?
O6 Re1 O4 80.55(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
O4 H4A O5 0.85(5) 1.80(5) 2.629(3) 164(5) 2_667 yes
O4 H4B F1 0.77(5) 2.46(5) 3.002(3) 128(4) 1_455 yes
O4 H4B O5 0.77(5) 2.09(5) 2.825(3) 160(5) 1_455 yes

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
C4 C5 C6 C7 -0.5(5) . . . . ?
C5 C4 N1 C8 0.5(5) . . . . ?
C5 C4 N1 Re1 -178.7(3) . . . . ?
C5 C6 C7 C8 0.3(5) . . . . ?
C5 C6 C7 F1 -179.2(3) . . . . ?
C6 C7 C8 C9 -178.0(3) . . . . ?
C6 C7 C8 N1 0.3(5) . . . . ?
C7 C8 C9 O5 2.6(4) . . . . ?
C7 C8 C9 O6 -177.4(3) . . . . ?
C7 C8 N1 C4 -0.7(4) . . . . ?
C7 C8 N1 Re1 178.6(2) . . . . ?
C8 C9 O6 Re1 -3.5(3) . . . . ?
C9 C8 N1 C4 177.8(3) . . . . ?
C9 C8 N1 Re1 -2.9(3) . . . . ?
F1 C7 C8 C9 1.5(5) . . . . ?
F1 C7 C8 N1 179.8(3) . . . . ?
N1 C4 C5 C6 0.1(6) . . . . ?
N1 C8 C9 O5 -175.8(2) . . . . ?
N1 C8 C9 O6 4.2(4) . . . . ?
O5 C9 O6 Re1 176.5(2) . . . . ?


####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 2205503'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O7 Re'
_chemical_formula_sum            'C10 H8 N O7 Re'
_chemical_formula_weight         440.37
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9487(3)
_cell_length_b                   6.8332(2)
_cell_length_c                   16.0682(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.801(3)
_cell_angle_gamma                90
_cell_volume                     1241.93(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10011
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.8100
_cell_measurement_theta_min      2.8870
_shelx_estimated_absorpt_T_max   0.697
_shelx_estimated_absorpt_T_min   0.077
_exptl_absorpt_coefficient_mu    19.455
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.1280
0 -1 0 0.1380
0 0 1 0.0311
0 0 -1 0.0391
-1 0 0 0.0085
1 0 0 0.0145

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02

_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11246
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.432
_diffrn_reflns_theta_min         3.908
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    104.00 177.00   0.50    0.30    --  107.75  45.00  60.00  146
  2  ω    136.00 171.00   0.50    0.30    --  107.75  45.00  90.00   70
  3  ω     95.00 133.00   0.50    0.30    --  107.75  45.00  90.00   76
  4  ω     29.00 125.00   0.50    0.15    --   51.79  77.00-150.00  192
  5  ω    -80.00  24.00   0.50    0.15    --  -51.79  89.00 158.00  208
  6  ω    -80.00 -10.00   0.50    0.30    --  -86.25  89.00 158.00  140
  7  ω   -162.00 -78.00   0.50    0.30    --  -86.25 -89.00  42.00  168
  8  ω   -126.00 -73.00   0.50    0.15    --  -51.79-125.00-180.00  106
  9  ω   -128.00 -78.00   0.50    0.15    --  -51.79 -89.00  42.00  100
 10  ω     32.00 120.00   0.50    0.30    --  107.75 -45.00 150.00  176
 11  ω     81.00 106.00   0.50    0.30    --  107.75 -94.00 120.00   50
 12  ω     31.00 106.00   0.50    0.30    --  107.75 -94.00  90.00  150
 13  ω    -21.00  80.00   0.50    0.15    --   51.79 -89.00  42.00  202
 14  ω     32.00 106.00   0.50    0.30    --  107.75 -89.00  42.00  148
 15  ω     34.00 130.00   0.50    0.30    --  107.75 -77.00 120.00  192
 16  ω     31.00 106.00   0.50    0.30    --  107.75 -94.00 -30.00  150
 17  ω     41.00  66.00   0.50    0.30    --  107.75 -94.00-180.00   50
 18  ω     73.00 105.00   0.50    0.30    --  107.75 -94.00-180.00   64
 19  ω    100.00 178.00   0.50    0.30    --  107.75  89.00 158.00  156
 20  ω    102.00 178.00   0.50    0.30    --  107.75 111.00 120.00  152
 21  ω    102.00 178.00   0.50    0.30    --  107.75 111.00   0.00  152
 22  ω    102.00 178.00   0.50    0.30    --  107.75 111.00-120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1285431000
_diffrn_orient_matrix_UB_12      -0.0344189000
_diffrn_orient_matrix_UB_13      0.0025775000
_diffrn_orient_matrix_UB_21      0.0350256000
_diffrn_orient_matrix_UB_22      0.2017196000
_diffrn_orient_matrix_UB_23      0.0432961000
_diffrn_orient_matrix_UB_31      0.0277758000
_diffrn_orient_matrix_UB_32      -0.0947405000
_diffrn_orient_matrix_UB_33      0.0914345000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2303
_reflns_number_total             2499

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.842
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.203
_refine_ls_extinction_coef       0.00116(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2499
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0574P)²+1.2329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0939
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.1718(3) 0.8895(5) 0.6495(2) 0.0276(7) Uani 1 1 d . . . . .
C2 C 0.3362(3) 0.9791(5) 0.5749(2) 0.0297(8) Uani 1 1 d . . . . .
C3 C 0.3661(3) 0.6673(5) 0.6765(2) 0.0265(7) Uani 1 1 d . . . . .
C4 C 0.3726(3) 0.6320(5) 0.4418(2) 0.0252(7) Uani 1 1 d . . . . .
H4 H 0.417082 0.748278 0.460888 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3923(3) 0.5222(5) 0.3759(2) 0.0278(7) Uani 1 1 d . . . . .
H5 H 0.450487 0.561870 0.350663 0.033 Uiso 1 1 calc R U . . .
C6 C 0.3274(3) 0.3549(6) 0.3467(2) 0.0301(8) Uani 1 1 d . . . . .
H6 H 0.340231 0.278909 0.301142 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2425(3) 0.2975(6) 0.3846(2) 0.0250(7) Uani 1 1 d . . . . .
C8 C 0.2276(3) 0.4138(5) 0.4526(2) 0.0200(6) Uani 1 1 d . . . . .
C9 C 0.1435(3) 0.3697(5) 0.5026(2) 0.0203(6) Uani 1 1 d . . . . .
C10 C 0.1784(5) 0.0287(7) 0.2858(3) 0.0537(13) Uani 1 1 d . . . . .
H10A H 0.156483 0.112652 0.233523 0.080 Uiso 1 1 calc R U . . .
H10B H 0.123622 -0.082198 0.275829 0.080 Uiso 1 1 calc R U . . .
H10C H 0.259089 -0.019928 0.297145 0.080 Uiso 1 1 calc R U . . .
N1 N 0.2926(2) 0.5789(4) 0.47951(17) 0.0207(5) Uani 1 1 d . . . . .
O1 O 0.1255(2) 0.9681(4) 0.69295(18) 0.0411(7) Uani 1 1 d . . . . .
O2 O 0.3943(2) 1.1130(4) 0.57265(19) 0.0429(7) Uani 1 1 d . . . . .
O3 O 0.4400(2) 0.6152(5) 0.73905(17) 0.0404(7) Uani 1 1 d . . . . .
O4 O 0.0991(2) 0.8257(4) 0.45511(15) 0.0219(5) Uani 1 1 d D . . . .
H4A H 0.042(3) 0.784(6) 0.468(4) 0.033 Uiso 1 1 d D U . . .
H4B H 0.104(4) 0.943(2) 0.445(3) 0.033 Uiso 1 1 d D U . . .
O5 O 0.0848(3) 0.2157(4) 0.4893(2) 0.0259(6) Uani 1 1 d . . . . .
O6 O 0.1398(2) 0.4958(3) 0.56017(15) 0.0221(5) Uani 1 1 d . . . . .
O7 O 0.1724(3) 0.1396(4) 0.36024(18) 0.0369(6) Uani 1 1 d . . . . .
Re1 Re 0.24347(2) 0.75228(2) 0.57540(2) 0.01872(14) 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
C1 O1 1.153(4) . ?
C1 Re1 1.920(4) . ?
C2 O2 1.156(4) . ?
C2 Re1 1.907(4) . ?
C3 O3 1.160(4) . ?
C3 Re1 1.894(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(5) . ?
C4 N1 1.337(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.376(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.396(5) . ?
C7 C8 1.408(5) . ?
C7 O7 1.345(5) . ?
C8 C9 1.505(4) . ?
C8 N1 1.358(4) . ?
C9 O5 1.244(4) . ?
C9 O6 1.275(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 O7 1.438(5) . ?
N1 Re1 2.169(3) . ?
O4 H4A 0.825(10) . ?
O4 H4B 0.822(10) . ?
O4 Re1 2.194(2) . ?
O6 Re1 2.114(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
O1 C1 Re1 177.8(3) . . ?
O2 C2 Re1 177.5(4) . . ?
O3 C3 Re1 178.9(3) . . ?
C5 C4 H4 119.2 . . ?
N1 C4 H4 119.2 . . ?
N1 C4 C5 121.6(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 120.2 . . ?
C5 C6 C7 119.6(3) . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C8 118.1(4) . . ?
O7 C7 C6 124.8(4) . . ?
O7 C7 C8 117.1(3) . . ?
C7 C8 C9 125.0(3) . . ?
N1 C8 C7 120.9(3) . . ?
N1 C8 C9 114.1(3) . . ?
O5 C9 C8 121.0(3) . . ?
O5 C9 O6 123.1(3) . . ?
O6 C9 C8 115.9(3) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C10 H10A 109.5 . . ?
O7 C10 H10B 109.5 . . ?
O7 C10 H10C 109.5 . . ?
C4 N1 C8 120.0(3) . . ?
C4 N1 Re1 124.8(2) . . ?
C8 N1 Re1 115.0(2) . . ?
H4A O4 H4B 120(4) . . ?
Re1 O4 H4A 100(4) . . ?
Re1 O4 H4B 108(3) . . ?
C9 O6 Re1 119.2(2) . . ?
C7 O7 C10 118.1(3) . . ?
C1 Re1 N1 169.71(12) . . ?
C1 Re1 O4 93.06(12) . . ?
C1 Re1 O6 96.59(12) . . ?
C2 Re1 C1 88.96(16) . . ?
C2 Re1 N1 98.65(14) . . ?
C2 Re1 O4 95.93(12) . . ?
C2 Re1 O6 173.14(12) . . ?
C3 Re1 C1 89.69(14) . . ?
C3 Re1 C2 87.85(16) . . ?
C3 Re1 N1 97.47(12) . . ?
C3 Re1 O4 175.36(13) . . ?
C3 Re1 O6 96.19(13) . . ?
N1 Re1 O4 79.34(9) . . ?
O6 Re1 N1 75.37(9) . . ?
O6 Re1 O4 79.80(9) . . ?

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
C5 H5 O3 0.95 2.54 3.270(4) 133.4 3_666 yes
O4 H4A O5 0.825(10) 1.854(19) 2.640(4) 159(4) 3_566 yes
O4 H4B O5 0.822(10) 2.03(3) 2.737(4) 143(4) 1_565 yes
O4 H4B O7 0.822(10) 2.25(3) 2.924(4) 140(4) 1_565 yes

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
C4 C5 C6 C7 -0.3(5) . . . . ?
C5 C4 N1 C8 -0.5(5) . . . . ?
C5 C4 N1 Re1 -174.4(2) . . . . ?
C5 C6 C7 C8 -0.7(6) . . . . ?
C5 C6 C7 O7 178.5(4) . . . . ?
C6 C7 C8 C9 -177.7(3) . . . . ?
C6 C7 C8 N1 1.1(5) . . . . ?
C6 C7 O7 C10 -4.8(6) . . . . ?
C7 C8 C9 O5 4.2(5) . . . . ?
C7 C8 C9 O6 -177.9(3) . . . . ?
C7 C8 N1 C4 -0.5(5) . . . . ?
C7 C8 N1 Re1 174.0(3) . . . . ?
C8 C7 O7 C10 174.5(4) . . . . ?
C8 C9 O6 Re1 2.5(4) . . . . ?
C9 C8 N1 C4 178.4(3) . . . . ?
C9 C8 N1 Re1 -7.0(3) . . . . ?
N1 C4 C5 C6 0.9(5) . . . . ?
N1 C8 C9 O5 -174.7(3) . . . . ?
N1 C8 C9 O6 3.2(4) . . . . ?
O5 C9 O6 Re1 -179.6(3) . . . . ?
O7 C7 C8 C9 3.0(5) . . . . ?
O7 C7 C8 N1 -178.2(3) . . . . ?


####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2205504'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C10 H5 F3 N O6 Re), 3(H2 O)'
_chemical_formula_sum            'C20 H16 F6 N2 O15 Re2'
_chemical_formula_weight         1010.75
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.2151(2)
_cell_length_b                   10.28390(10)
_cell_length_c                   11.55570(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.5060(10)
_cell_angle_gamma                90
_cell_volume                     2877.55(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13258
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3560
_cell_measurement_theta_min      3.6320
_shelx_estimated_absorpt_T_max   0.182
_shelx_estimated_absorpt_T_min   0.070
_exptl_absorpt_coefficient_mu    17.251
_exptl_absorpt_correction_T_max  0.238
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0746
-1 0 0 0.0746
-1 -5 -1 0.1226
0 0 -1 0.0864
5 -3 4 0.1133
5 5 3 0.1099
-5 -3 2 0.0948
-5 4 2 0.1399
2 -1 5 0.1339
-5 -1 -1 0.0965

_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15

_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14283
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.651
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -16.00   1.00    1.00    --  -42.49 -57.00  30.00   97
  2  ω    -87.00  -6.00   1.00    1.00    --  -42.49 125.00  90.00   81
  3  ω    -87.00  -6.00   1.00    1.00    --  -42.49 125.00 150.00   81
  4  ω     20.00 115.00   1.00    1.00    --   42.49  37.00 -60.00   95
  5  ω      6.00  82.00   1.00    1.00    --   42.49 -99.00  60.00   76
  6  ω     87.00 178.00   1.00    2.00    --  111.00  45.00-180.00   91
  7  ω     36.00 109.00   1.00    2.00    --  111.00-111.00  30.00   73
  8  ω     30.00 107.00   1.00    2.00    --  111.00 -94.00 -90.00   77
  9  ω     40.00 135.00   1.00    2.00    --  111.00 -45.00-120.00   95
 10  ω    103.00 178.00   1.00    2.00    --  111.00  77.00 -90.00   75
 11  ω    103.00 178.00   1.00    2.00    --  111.00  77.00-120.00   75
 12  ω     36.00 109.00   1.00    2.00    --  111.00-111.00-120.00   73
 13  ω    103.00 178.00   1.00    2.00    --  111.00  77.00 -30.00   75
 14  ω     83.00 178.00   1.00    2.00    --  111.00  61.00-120.00   95
 15  ω     36.00 109.00   1.00    2.00    --  111.00-111.00 -30.00   73
 16  ω     36.00 135.00   1.00    2.00    --  111.00 -30.00  90.00   99
 17  ω    104.00 178.00   1.00    2.00    --  111.00 111.00  60.00   74
 18  ω     87.00 178.00   1.00    2.00    --  111.00  30.00 -30.00   91
 19  ω   -113.00 -16.00   1.00    1.00    --  -42.49 -57.00 150.00   97
 20  ω   -113.00 -27.00   1.00    1.00    --  -42.49 -57.00 -60.00   86
 21  ω    -30.00  65.00   1.00    1.00    --   42.49 -37.00-120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0553194000
_diffrn_orient_matrix_UB_12      -0.0733448000
_diffrn_orient_matrix_UB_13      -0.0092206000
_diffrn_orient_matrix_UB_21      -0.0002656000
_diffrn_orient_matrix_UB_22      0.0192063000
_diffrn_orient_matrix_UB_23      -0.1322497000
_diffrn_orient_matrix_UB_31      0.0314161000
_diffrn_orient_matrix_UB_32      -0.1291443000
_diffrn_orient_matrix_UB_33      -0.0145928000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2936
_reflns_number_total             2953

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.122
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.000380(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2953
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²+14.4789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0652
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.66638(18) 0.4303(4) 0.7424(4) 0.0316(9) Uani 1 1 d . . . . .
C2 C 0.69155(17) 0.6534(4) 0.8413(4) 0.0330(9) Uani 1 1 d . . . . .
C3 C 0.73094(19) 0.5953(4) 0.6323(4) 0.0319(9) Uani 1 1 d . . . . .
C4 C 0.66825(17) 0.9120(4) 0.6662(4) 0.0270(8) Uani 1 1 d . . . . .
H4 H 0.693498 0.906554 0.729452 0.032 Uiso 1 1 calc R U . . .
C5 C 0.65684(17) 1.0316(4) 0.6191(4) 0.0313(9) Uani 1 1 d . . . . .
H5 H 0.674043 1.107663 0.649042 0.038 Uiso 1 1 calc R U . . .
C6 C 0.62009(16) 1.0397(4) 0.5278(4) 0.0294(8) Uani 1 1 d . . . . .
H6 H 0.611516 1.121811 0.494571 0.035 Uiso 1 1 calc R U . . .
C7 C 0.59554(15) 0.9274(4) 0.4842(3) 0.0239(7) Uani 1 1 d . . . . .
C8 C 0.60842(14) 0.8092(4) 0.5368(3) 0.0209(7) Uani 1 1 d . . . . .
C9 C 0.58493(15) 0.6770(4) 0.5024(3) 0.0211(7) Uani 1 1 d . . . . .
C10 C 0.55720(18) 0.9386(4) 0.3803(4) 0.0318(9) Uani 1 1 d . . . . .
F1 F 0.50475(11) 0.9145(3) 0.4048(3) 0.0399(6) Uani 1 1 d . . . . .
F2 F 0.55899(15) 1.0603(3) 0.3380(3) 0.0551(8) Uani 1 1 d . . . . .
F3 F 0.57218(13) 0.8611(3) 0.2938(2) 0.0389(6) Uani 1 1 d . . . . .
N1 N 0.64477(12) 0.8017(3) 0.6258(3) 0.0217(6) Uani 1 1 d . . . . .
O1 O 0.67218(17) 0.3243(3) 0.7705(4) 0.0520(9) Uani 1 1 d . . . . .
O2 O 0.71013(17) 0.6800(5) 0.9300(3) 0.0569(10) Uani 1 1 d . . . . .
O3 O 0.77471(14) 0.5875(4) 0.5942(4) 0.0492(9) Uani 1 1 d . . . . .
O4 O 0.57506(12) 0.6397(3) 0.7542(3) 0.0236(5) Uani 1 1 d . . . . .
H4A H 0.558(2) 0.579(5) 0.736(4) 0.025(12) Uiso 1 1 d . . . . .
H4B H 0.577(3) 0.660(7) 0.814(6) 0.047(18) Uiso 1 1 d . . . . .
O5 O 0.54324(12) 0.6706(3) 0.4416(2) 0.0301(6) Uani 1 1 d . . . . .
O6 O 0.61130(11) 0.5786(3) 0.5421(2) 0.0237(5) Uani 1 1 d . . . . .
O7 O 0.500000 0.4458(4) 0.750000 0.0248(8) Uani 1 2 d S T P . .
H7 H 0.488(2) 0.399(5) 0.697(5) 0.034(14) Uiso 1 1 d . . . . .
O8 O 0.56945(13) 0.3345(3) 0.4805(2) 0.0252(6) Uani 1 1 d . . . . .
H8A H 0.578(2) 0.402(6) 0.504(5) 0.033(15) Uiso 1 1 d . . . . .
H8B H 0.539(3) 0.327(6) 0.509(5) 0.038(15) Uiso 1 1 d . . . . .
Re1 Re 0.65936(2) 0.60861(2) 0.69564(2) 0.01948(9) 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
C1 O1 1.145(6) . ?
C1 Re1 1.919(4) . ?
C2 O2 1.148(6) . ?
C2 Re1 1.906(4) . ?
C3 O3 1.154(6) . ?
C3 Re1 1.892(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(6) . ?
C4 N1 1.350(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(6) . ?
C7 C8 1.393(5) . ?
C7 C10 1.516(6) . ?
C8 C9 1.525(5) . ?
C8 N1 1.350(5) . ?
C9 O5 1.226(5) . ?
C9 O6 1.280(5) . ?
C10 F1 1.327(5) . ?
C10 F2 1.344(5) . ?
C10 F3 1.332(5) . ?
N1 Re1 2.171(3) . ?
O4 H4A 0.77(6) . ?
O4 H4B 0.72(7) . ?
O4 Re1 2.180(3) . ?
O6 Re1 2.136(3) . ?
O7 H7 0.83(5) 2_656 ?
O7 H7 0.83(5) . ?
O8 H8A 0.77(6) . ?
O8 H8B 0.82(6) . ?

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
O1 C1 Re1 178.0(4) . . ?
O2 C2 Re1 178.9(4) . . ?
O3 C3 Re1 179.6(5) . . ?
C5 C4 H4 118.9 . . ?
N1 C4 H4 118.9 . . ?
N1 C4 C5 122.2(4) . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.9(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 118.3(4) . . ?
C6 C7 C10 118.7(4) . . ?
C8 C7 C10 123.0(4) . . ?
C7 C8 C9 125.6(3) . . ?
N1 C8 C7 121.6(3) . . ?
N1 C8 C9 112.8(3) . . ?
O5 C9 C8 120.0(3) . . ?
O5 C9 O6 124.6(4) . . ?
O6 C9 C8 115.3(3) . . ?
F1 C10 C7 113.4(3) . . ?
F1 C10 F2 106.6(4) . . ?
F1 C10 F3 108.4(4) . . ?
F2 C10 C7 109.7(4) . . ?
F3 C10 C7 112.3(3) . . ?
F3 C10 F2 105.9(4) . . ?
C4 N1 Re1 124.9(3) . . ?
C8 N1 C4 119.1(3) . . ?
C8 N1 Re1 116.0(2) . . ?
H4A O4 H4B 122(6) . . ?
Re1 O4 H4A 106(4) . . ?
Re1 O4 H4B 106(5) . . ?
C9 O6 Re1 116.8(2) . . ?
H7 O7 H7 109(7) . 2_656 ?
H8A O8 H8B 100(6) . . ?
C1 Re1 N1 172.93(15) . . ?
C1 Re1 O4 97.69(16) . . ?
C1 Re1 O6 98.17(15) . . ?
C2 Re1 C1 87.0(2) . . ?
C2 Re1 N1 99.87(16) . . ?
C2 Re1 O4 93.84(16) . . ?
C2 Re1 O6 169.93(15) . . ?
C3 Re1 C1 87.74(19) . . ?
C3 Re1 C2 89.4(2) . . ?
C3 Re1 N1 93.95(16) . . ?
C3 Re1 O4 173.79(16) . . ?
C3 Re1 O6 99.35(16) . . ?
N1 Re1 O4 80.30(11) . . ?
O6 Re1 N1 74.78(11) . . ?
O6 Re1 O4 76.96(11) . . ?

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
C4 C5 C6 C7 -0.5(6) . . . . ?
C5 C4 N1 C8 -0.7(6) . . . . ?
C5 C4 N1 Re1 -179.2(3) . . . . ?
C5 C6 C7 C8 1.2(6) . . . . ?
C5 C6 C7 C10 -177.3(4) . . . . ?
C6 C7 C8 C9 178.9(3) . . . . ?
C6 C7 C8 N1 -1.7(5) . . . . ?
C6 C7 C10 F1 -111.4(4) . . . . ?
C6 C7 C10 F2 7.6(5) . . . . ?
C6 C7 C10 F3 125.2(4) . . . . ?
C7 C8 C9 O5 -16.6(5) . . . . ?
C7 C8 C9 O6 164.1(3) . . . . ?
C7 C8 N1 C4 1.5(5) . . . . ?
C7 C8 N1 Re1 -179.9(3) . . . . ?
C8 C7 C10 F1 70.1(5) . . . . ?
C8 C7 C10 F2 -170.8(4) . . . . ?
C8 C7 C10 F3 -53.3(5) . . . . ?
C8 C9 O6 Re1 24.0(4) . . . . ?
C9 C8 N1 C4 -179.1(3) . . . . ?
C9 C8 N1 Re1 -0.5(4) . . . . ?
C10 C7 C8 C9 -2.6(6) . . . . ?
C10 C7 C8 N1 176.8(3) . . . . ?
N1 C4 C5 C6 0.2(6) . . . . ?
N1 C8 C9 O5 164.0(3) . . . . ?
N1 C8 C9 O6 -15.3(4) . . . . ?
O5 C9 O6 Re1 -155.3(3) . . . . ?


####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 2205506'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-12
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 Cl N O6 Re'
_chemical_formula_sum            'C9 H5 Cl N O6 Re'
_chemical_formula_weight         444.79
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   9.33670(10)
_cell_length_b                   11.12590(10)
_cell_length_c                   22.2200(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.6720(10)
_cell_angle_gamma                90
_cell_volume                     2275.39(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    11234
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      79.0280
_cell_measurement_theta_min      3.9950
_shelx_estimated_absorpt_T_max   0.456
_shelx_estimated_absorpt_T_min   0.184
_exptl_absorpt_coefficient_mu    23.293
_exptl_absorpt_correction_T_max  0.467
_exptl_absorpt_correction_T_min  0.200
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0209
-1 1 0 0.0209
0 0 -1 0.0360
0 0 1 0.0360
1 1 0 0.0526
-1 -1 0 0.0426
-1 1 5 0.0353
-1 1 -5 0.0306

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04

_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11613
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.487
_diffrn_reflns_theta_min         4.036
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     92.00 178.00   0.50    1.20    --  107.75  61.00 -30.00  172
  2  ω     94.00 178.00   0.50    1.20    --  107.75  30.00   0.00  168
  3  ω     96.00 178.00   0.50    1.20    --  107.75  15.00 -30.00  164
  4  ω     91.00 178.00   0.50    1.20    --  107.75  64.00  45.00  174
  5  ω    129.00 178.00   0.50    1.20    --  107.75  15.00 150.00   98
  6  ω     96.00 178.00   0.50    1.20    --  107.75  15.00 120.00  164
  7  ω     96.00 178.00   0.50    1.20    --  107.75  15.00  90.00  164
  8  ω     85.00 178.00   0.50    1.20    --  107.75  77.00 120.00  186
  9  ω     32.00 120.00   0.50    1.20    --  107.75 -45.00  60.00  176
 10  ω    -18.00  69.00   0.50    0.30    --   51.79 -64.00 -90.00  174
 11  ω     38.00 125.00   0.50    1.20    --  107.75 -64.00 -90.00  174
 12  ω    102.00 178.00   0.50    1.20    --  107.75 111.00 -30.00  152
 13  ω     31.00 109.00   0.50    1.20    --  107.75-111.00  60.00  156
 14  ω     36.00 101.00   0.50    1.20    --  107.75 -94.00 120.00  130
 15  ω   -122.00 -35.00   0.50    0.30    --  -51.79 -64.00 -90.00  174
 16  ω   -126.00 -73.00   0.50    0.30    --  -51.79-125.00   0.00  106
 17  ω   -126.00 -73.00   0.50    0.30    --  -51.79-125.00  90.00  106
 18  ω    -69.00  18.00   0.50    0.30    --  -51.79  64.00  45.00  174
 19  ω   -103.00 -16.00   0.50    1.20    --  -86.25  64.00  45.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0647678000
_diffrn_orient_matrix_UB_12      -0.0953672000
_diffrn_orient_matrix_UB_13      -0.0379284000
_diffrn_orient_matrix_UB_21      -0.1049369000
_diffrn_orient_matrix_UB_22      0.0401900000
_diffrn_orient_matrix_UB_23      -0.0575511000
_diffrn_orient_matrix_UB_31      0.1132209000
_diffrn_orient_matrix_UB_32      0.0918837000
_diffrn_orient_matrix_UB_33      -0.0141372000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2309
_reflns_number_total             2318

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.000335(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0134
_refine_ls_restrained_S_all      1.289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0136P)²+4.7286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0336
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.5396(3) 0.5734(2) 0.32957(12) 0.0217(5) Uani 1 1 d . . . . .
C2 C 0.3911(3) 0.3810(2) 0.28507(12) 0.0178(5) Uani 1 1 d . . . . .
C3 C 0.6609(3) 0.3904(2) 0.27475(12) 0.0177(5) Uani 1 1 d . . . . .
C4 C 0.5375(3) 0.1187(2) 0.34463(11) 0.0183(5) Uani 1 1 d . . . . .
H4 H 0.451456 0.130139 0.315631 0.022 Uiso 1 1 calc R U . . .
C5 C 0.5811(3) 0.0026(2) 0.36064(12) 0.0196(5) Uani 1 1 d . . . . .
H5 H 0.525929 -0.064404 0.343314 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7080(3) -0.0136(2) 0.40284(11) 0.0204(5) Uani 1 1 d . . . . .
C7 C 0.7853(3) 0.0854(2) 0.42818(12) 0.0195(5) Uani 1 1 d . . . . .
H7 H 0.871665 0.076246 0.457236 0.023 Uiso 1 1 calc R U . . .
C8 C 0.7326(3) 0.1986(2) 0.40983(11) 0.0165(4) Uani 1 1 d . . . . .
C9 C 0.8102(3) 0.3110(2) 0.43584(11) 0.0181(5) Uani 1 1 d . . . . .
Cl1 Cl 0.76971(8) -0.15628(6) 0.42250(3) 0.02915(14) Uani 1 1 d . . . . .
N1 N 0.6116(2) 0.21601(18) 0.36837(9) 0.0152(4) Uani 1 1 d . . . . .
O1 O 0.5231(2) 0.67430(17) 0.32121(10) 0.0307(4) Uani 1 1 d . . . . .
O2 O 0.2901(2) 0.36872(17) 0.24841(9) 0.0254(4) Uani 1 1 d . . . . .
O3 O 0.7121(2) 0.38000(18) 0.23123(9) 0.0252(4) Uani 1 1 d . . . . .
O4 O 0.4516(2) 0.40407(17) 0.42175(9) 0.0205(4) Uani 1 1 d . . . . .
H4A H 0.493(4) 0.381(3) 0.455(2) 0.032(10) Uiso 1 1 d . . . . .
H4B H 0.401(4) 0.455(4) 0.4240(17) 0.030(10) Uiso 1 1 d . . . . .
O5 O 0.91660(19) 0.30113(17) 0.47621(9) 0.0246(4) Uani 1 1 d . . . . .
O6 O 0.75570(19) 0.41045(15) 0.41283(8) 0.0186(4) Uani 1 1 d . . . . .
Re1 Re 0.56429(2) 0.40289(2) 0.34294(2) 0.01436(5) 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
C1 O1 1.144(3) . ?
C1 Re1 1.928(3) . ?
C2 O2 1.146(3) . ?
C2 Re1 1.905(3) . ?
C3 O3 1.155(3) . ?
C3 Re1 1.894(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(4) . ?
C4 N1 1.345(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(4) . ?
C6 C7 1.384(4) . ?
C6 Cl1 1.720(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(3) . ?
C8 C9 1.510(3) . ?
C8 N1 1.346(3) . ?
C9 O5 1.227(3) . ?
C9 O6 1.287(3) . ?
N1 Re1 2.180(2) . ?
O4 H4A 0.81(4) . ?
O4 H4B 0.75(4) . ?
O4 Re1 2.1890(19) . ?
O6 Re1 2.1633(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 179.1(3) . . ?
O2 C2 Re1 177.2(2) . . ?
O3 C3 Re1 175.9(2) . . ?
C5 C4 H4 118.6 . . ?
N1 C4 H4 118.6 . . ?
N1 C4 C5 122.8(2) . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.3(2) . . ?
C6 C5 H5 120.8 . . ?
C5 C6 Cl1 120.1(2) . . ?
C7 C6 C5 119.8(2) . . ?
C7 C6 Cl1 120.1(2) . . ?
C6 C7 H7 121.0 . . ?
C6 C7 C8 117.9(2) . . ?
C8 C7 H7 121.0 . . ?
C7 C8 C9 121.0(2) . . ?
N1 C8 C7 123.1(2) . . ?
N1 C8 C9 115.9(2) . . ?
O5 C9 C8 118.9(2) . . ?
O5 C9 O6 125.8(2) . . ?
O6 C9 C8 115.3(2) . . ?
C4 N1 C8 118.1(2) . . ?
C4 N1 Re1 126.71(17) . . ?
C8 N1 Re1 115.12(16) . . ?
H4A O4 H4B 113(4) . . ?
Re1 O4 H4A 120(3) . . ?
Re1 O4 H4B 117(3) . . ?
C9 O6 Re1 118.37(15) . . ?
C1 Re1 N1 172.76(9) . . ?
C1 Re1 O4 93.22(9) . . ?
C1 Re1 O6 97.78(9) . . ?
C2 Re1 C1 87.48(11) . . ?
C2 Re1 N1 99.49(9) . . ?
C2 Re1 O4 94.20(9) . . ?
C2 Re1 O6 174.09(8) . . ?
C3 Re1 C1 90.55(11) . . ?
C3 Re1 C2 85.11(11) . . ?
C3 Re1 N1 91.96(9) . . ?
C3 Re1 O4 176.13(9) . . ?
C3 Re1 O6 97.48(9) . . ?
N1 Re1 O4 84.39(7) . . ?
O6 Re1 N1 75.17(7) . . ?
O6 Re1 O4 82.85(7) . . ?

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
O4 H4A O5 0.81(4) 1.85(4) 2.651(3) 170(4) 2_656 yes
O4 H4B O6 0.75(4) 2.01(4) 2.743(3) 169(4) 6_565 yes

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
C4 C5 C6 C7 1.0(4) . . . . ?
C4 C5 C6 Cl1 -178.06(19) . . . . ?
C5 C4 N1 C8 -0.6(4) . . . . ?
C5 C4 N1 Re1 175.50(18) . . . . ?
C5 C6 C7 C8 -0.5(4) . . . . ?
C6 C7 C8 C9 179.5(2) . . . . ?
C6 C7 C8 N1 -0.7(4) . . . . ?
C7 C8 C9 O5 -4.0(3) . . . . ?
C7 C8 C9 O6 176.3(2) . . . . ?
C7 C8 N1 C4 1.2(3) . . . . ?
C7 C8 N1 Re1 -175.32(18) . . . . ?
C8 C9 O6 Re1 0.8(3) . . . . ?
C9 C8 N1 C4 -178.9(2) . . . . ?
C9 C8 N1 Re1 4.5(3) . . . . ?
Cl1 C6 C7 C8 178.63(18) . . . . ?
N1 C4 C5 C6 -0.5(4) . . . . ?
N1 C8 C9 O5 176.1(2) . . . . ?
N1 C8 C9 O6 -3.6(3) . . . . ?
O5 C9 O6 Re1 -178.87(19) . . . . ?


####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 2205507'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 F N O6 Re'
_chemical_formula_sum            'C9 H5 F N O6 Re'
_chemical_formula_weight         428.34
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.0882(2)
_cell_length_b                   19.6105(3)
_cell_length_c                   12.6146(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.846(3)
_cell_angle_gamma                90
_cell_volume                     2299.81(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16882
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.5160
_cell_measurement_theta_min      2.2120
_shelx_estimated_absorpt_T_max   0.365
_shelx_estimated_absorpt_T_min   0.059
_exptl_absorpt_coefficient_mu    21.048
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.025
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -1 0.0314
-1 -1 1 0.0314
-1 0 1 0.0216
1 0 -1 0.0456
1 -1 2 0.1506
-1 1 -2 0.1506
0 -1 0 0.0442
0 1 0 0.0602
-5 -7 4 0.0277
2 5 -2 0.0406
-2 5 1 0.0472
-1 11 5 0.0870
3 9 2 0.1022
2 -12 -3 0.0381

_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06

_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21410
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.234
_diffrn_reflns_theta_min         4.421
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  35.00   1.00    1.00    --  -40.76  37.00   0.00  102
  2  ω   -117.00 -14.00   1.00    1.00    --  -40.76 -37.00-180.00  103
  3  ω     11.00 115.00   1.00    1.00    --   40.76  57.00 150.00  104
  4  ω      6.00  83.00   1.00    1.00    --   40.76 -99.00  30.00   77
  5  ω     39.00 143.00   1.00    1.50    --  113.00 -61.00 -90.00  104
  6  ω     38.00 141.00   1.00    1.50    --  113.00 -45.00-120.00  103
  7  ω     83.00 178.00   1.00    1.50    --  113.00  61.00  60.00   95
  8  ω     35.00 109.00   1.00    1.50    --  113.00-111.00-180.00   74
  9  ω    104.00 178.00   1.00    1.50    --  113.00 111.00-120.00   74
 10  ω     85.00 178.00   1.00    1.50    --  113.00  45.00 -30.00   93
 11  ω    103.00 178.00   1.00    1.50    --  113.00  77.00 -30.00   75
 12  ω     29.00 107.00   1.00    1.50    --  113.00 -94.00 -60.00   78
 13  ω     35.00 109.00   1.00    1.50    --  113.00-111.00   0.00   74
 14  ω    103.00 178.00   1.00    1.50    --  113.00  77.00  30.00   75
 15  ω    103.00 178.00   1.00    1.50    --  113.00  77.00 120.00   75
 16  ω   -117.00 -14.00   1.00    1.00    --  -40.76 -37.00  30.00  103
 17  ω   -115.00 -11.00   1.00    1.00    --  -40.76 -57.00 -30.00  104
 18  ω      6.00  83.00   1.00    1.00    --   40.76 -99.00-180.00   77
 19  ω     83.00 108.00   1.00    1.50    --  113.00  61.00 -90.00   25
 20  ω     52.00 178.00   1.00    1.50    --  113.00  15.00-180.00  126
 21  ω     82.00 178.00   1.00    1.50    --  113.00  30.00-120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1243778000
_diffrn_orient_matrix_UB_12      -0.0475162000
_diffrn_orient_matrix_UB_13      -0.0713055000
_diffrn_orient_matrix_UB_21      -0.1069905000
_diffrn_orient_matrix_UB_22      0.0458575000
_diffrn_orient_matrix_UB_23      0.0270937000
_diffrn_orient_matrix_UB_31      -0.0233751000
_diffrn_orient_matrix_UB_32      0.0425587000
_diffrn_orient_matrix_UB_33      -0.1082794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4208
_reflns_number_total             4214

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.000277(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.276
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+9.4794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0629
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C13(H13), C14(H14), C16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.8838(6) 0.6171(3) 1.2731(5) 0.0375(14) Uani 1 1 d . . . . .
H4A H 0.815(9) 0.499(4) 1.388(7) 0.056 Uiso 1 1 d . U . . .
H4B H 0.812(8) 0.522(4) 1.484(7) 0.056 Uiso 1 1 d . U . . .
H10A H 0.335(8) 0.516(4) 0.979(7) 0.056 Uiso 1 1 d . U . . .
H10B H 0.355(9) 0.485(4) 0.888(7) 0.056 Uiso 1 1 d . U . . .
C2 C 0.8798(6) 0.6655(3) 1.4712(5) 0.0350(13) Uani 1 1 d . . . . .
C3 C 0.7047(7) 0.7157(3) 1.2728(5) 0.0377(14) Uani 1 1 d . . . . .
C4 C 0.5525(6) 0.6589(3) 1.4777(4) 0.0321(12) Uani 1 1 d . . . . .
H4 H 0.636012 0.681303 1.529553 0.039 Uiso 1 1 calc R U . . .
C5 C 0.4308(6) 0.6584(3) 1.5018(5) 0.0337(12) Uani 1 1 d . . . . .
H5 H 0.428594 0.681449 1.567328 0.040 Uiso 1 1 calc R U . . .
C6 C 0.3117(7) 0.6233(3) 1.4280(5) 0.0347(12) Uani 1 1 d . . . . .
C7 C 0.3127(6) 0.5925(3) 1.3296(4) 0.0311(11) Uani 1 1 d . . . . .
H7 H 0.230819 0.569141 1.277581 0.037 Uiso 1 1 calc R U . . .
C8 C 0.4380(6) 0.5974(3) 1.3106(4) 0.0250(10) Uani 1 1 d . . . . .
C9 C 0.4502(6) 0.5682(3) 1.2035(4) 0.0247(10) Uani 1 1 d . . . . .
C10 C 0.4475(6) 0.5901(3) 0.7633(4) 0.0295(12) Uani 1 1 d . . . . .
C11 C 0.4537(6) 0.6559(3) 0.9499(5) 0.0297(11) Uani 1 1 d . . . . .
C12 C 0.2843(6) 0.6979(3) 0.7481(4) 0.0298(11) Uani 1 1 d . . . . .
C13 C 0.1312(6) 0.6580(3) 0.9744(4) 0.0281(11) Uani 1 1 d . . . . .
H13 H 0.216375 0.681496 1.020689 0.034 Uiso 1 1 calc R U . . .
C14 C 0.0158(6) 0.6582(3) 1.0078(5) 0.0332(12) Uani 1 1 d . . . . .
H14 H 0.020730 0.681507 1.075307 0.040 Uiso 1 1 calc R U . . .
C15 C -0.1051(7) 0.6239(3) 0.9406(5) 0.0371(13) Uani 1 1 d . . . . .
C16 C -0.1146(6) 0.5901(3) 0.8416(5) 0.0355(13) Uani 1 1 d . . . . .
H16 H -0.199156 0.566463 0.794519 0.043 Uiso 1 1 calc R U . . .
C17 C 0.0052(6) 0.5928(3) 0.8156(4) 0.0262(10) Uani 1 1 d . . . . .
C18 C 0.0074(6) 0.5586(3) 0.7079(4) 0.0275(11) Uani 1 1 d . . . . .
F1 F 0.1950(4) 0.6199(2) 1.4537(3) 0.0525(10) Uani 1 1 d . . . . .
F2 F -0.2202(4) 0.6228(2) 0.9699(3) 0.0540(11) Uani 1 1 d . . . . .
N1 N 0.5578(5) 0.6291(2) 1.3835(3) 0.0263(9) Uani 1 1 d . . . . .
N2 N 0.1281(5) 0.6259(2) 0.8792(4) 0.0236(9) Uani 1 1 d . . . . .
O1 O 0.9647(5) 0.6119(3) 1.2272(4) 0.0588(14) Uani 1 1 d . . . . .
O2 O 0.9607(5) 0.6892(2) 1.5555(4) 0.0477(11) Uani 1 1 d . . . . .
O3 O 0.6865(6) 0.7705(2) 1.2378(4) 0.0550(14) Uani 1 1 d . . . . .
O4 O 0.7660(4) 0.52454(19) 1.4129(3) 0.0262(7) Uani 1 1 d . . . . .
O5 O 0.3444(4) 0.54272(19) 1.1278(3) 0.0287(8) Uani 1 1 d . . . . .
O6 O 0.5753(4) 0.57315(17) 1.1994(3) 0.0251(7) Uani 1 1 d . . . . .
O7 O 0.5300(4) 0.5782(2) 0.7240(3) 0.0355(9) Uani 1 1 d . . . . .
O8 O 0.5430(5) 0.6843(2) 1.0242(3) 0.0400(10) Uani 1 1 d . . . . .
O9 O 0.2779(5) 0.7502(2) 0.7033(4) 0.0429(10) Uani 1 1 d . . . . .
O10 O 0.3129(4) 0.51522(19) 0.9106(3) 0.0257(8) Uani 1 1 d . . . . .
O11 O -0.1025(4) 0.5312(2) 0.6414(3) 0.0361(9) Uani 1 1 d . . . . .
O12 O 0.1276(4) 0.56205(18) 0.6957(3) 0.0260(7) Uani 1 1 d . . . . .
Re1 Re 0.74148(2) 0.62642(2) 1.33605(2) 0.02574(8) Uani 1 1 d . . . . .
Re2 Re 0.30500(2) 0.61329(2) 0.82458(2) 0.02189(8) 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
C1 O1 1.174(8) . ?
C1 Re1 1.900(6) . ?
C2 O2 1.157(7) . ?
C2 Re1 1.896(6) . ?
C3 O3 1.150(7) . ?
C3 Re1 1.899(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.374(8) . ?
C4 N1 1.345(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(8) . ?
C6 C7 1.384(8) . ?
C6 F1 1.337(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.379(8) . ?
C8 C9 1.515(7) . ?
C8 N1 1.352(7) . ?
C9 O5 1.229(6) . ?
C9 O6 1.287(6) . ?
C10 O7 1.145(7) . ?
C10 Re2 1.933(6) . ?
C11 O8 1.159(7) . ?
C11 Re2 1.899(6) . ?
C12 O9 1.160(7) . ?
C12 Re2 1.890(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(8) . ?
C13 N2 1.346(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.364(9) . ?
C15 C16 1.382(8) . ?
C15 F2 1.348(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.371(8) . ?
C17 C18 1.522(7) . ?
C17 N2 1.353(7) . ?
C18 O11 1.224(6) . ?
C18 O12 1.282(7) . ?
N1 Re1 2.157(5) . ?
N2 Re2 2.162(4) . ?
O4 H4A 0.84(8) . ?
O4 H4B 0.84(8) . ?
O4 Re1 2.193(4) . ?
O6 Re1 2.152(3) . ?
O10 H10A 0.80(8) . ?
O10 H10B 0.84(9) . ?
O10 Re2 2.195(4) . ?
O12 Re2 2.144(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 175.6(5) . . ?
O2 C2 Re1 177.5(6) . . ?
O3 C3 Re1 177.6(5) . . ?
C5 C4 H4 118.7 . . ?
N1 C4 H4 118.7 . . ?
N1 C4 C5 122.5(5) . . ?
C4 C5 H5 120.9 . . ?
C4 C5 C6 118.2(5) . . ?
C6 C5 H5 120.9 . . ?
C7 C6 C5 120.8(6) . . ?
F1 C6 C5 118.6(5) . . ?
F1 C6 C7 120.6(5) . . ?
C6 C7 H7 121.5 . . ?
C8 C7 C6 116.9(5) . . ?
C8 C7 H7 121.5 . . ?
C7 C8 C9 121.7(5) . . ?
N1 C8 C7 123.5(5) . . ?
N1 C8 C9 114.8(5) . . ?
O5 C9 C8 120.0(5) . . ?
O5 C9 O6 124.6(5) . . ?
O6 C9 C8 115.3(4) . . ?
O7 C10 Re2 177.5(5) . . ?
O8 C11 Re2 177.4(5) . . ?
O9 C12 Re2 177.1(5) . . ?
C14 C13 H13 118.5 . . ?
N2 C13 H13 118.5 . . ?
N2 C13 C14 122.9(5) . . ?
C13 C14 H14 121.2 . . ?
C15 C14 C13 117.6(5) . . ?
C15 C14 H14 121.2 . . ?
C14 C15 C16 122.0(6) . . ?
F2 C15 C14 119.6(5) . . ?
F2 C15 C16 118.4(6) . . ?
C15 C16 H16 122.0 . . ?
C17 C16 C15 116.1(5) . . ?
C17 C16 H16 122.0 . . ?
C16 C17 C18 121.1(5) . . ?
N2 C17 C16 124.5(5) . . ?
N2 C17 C18 114.4(5) . . ?
O11 C18 C17 118.8(5) . . ?
O11 C18 O12 126.0(5) . . ?
O12 C18 C17 115.2(4) . . ?
C4 N1 C8 117.9(5) . . ?
C4 N1 Re1 126.1(4) . . ?
C8 N1 Re1 116.0(3) . . ?
C13 N2 C17 116.9(5) . . ?
C13 N2 Re2 127.0(4) . . ?
C17 N2 Re2 115.9(3) . . ?
H4A O4 H4B 102(7) . . ?
Re1 O4 H4A 111(5) . . ?
Re1 O4 H4B 117(5) . . ?
C9 O6 Re1 118.4(3) . . ?
H10A O10 H10B 114(8) . . ?
Re2 O10 H10A 118(6) . . ?
Re2 O10 H10B 112(5) . . ?
C18 O12 Re2 118.9(3) . . ?
C1 Re1 N1 171.0(2) . . ?
C1 Re1 O4 97.1(2) . . ?
C1 Re1 O6 95.6(2) . . ?
C2 Re1 C1 90.2(3) . . ?
C2 Re1 C3 87.7(2) . . ?
C2 Re1 N1 98.8(2) . . ?
C2 Re1 O4 93.08(19) . . ?
C2 Re1 O6 171.6(2) . . ?
C3 Re1 C1 88.3(3) . . ?
C3 Re1 N1 92.6(2) . . ?
C3 Re1 O4 174.6(2) . . ?
C3 Re1 O6 98.42(19) . . ?
N1 Re1 O4 82.01(15) . . ?
O6 Re1 N1 75.40(15) . . ?
O6 Re1 O4 80.27(14) . . ?
C10 Re2 N2 171.36(19) . . ?
C10 Re2 O10 95.88(18) . . ?
C10 Re2 O12 96.78(18) . . ?
C11 Re2 C10 88.1(2) . . ?
C11 Re2 N2 99.6(2) . . ?
C11 Re2 O10 96.26(18) . . ?
C11 Re2 O12 174.02(19) . . ?
C12 Re2 C10 87.3(2) . . ?
C12 Re2 C11 86.2(2) . . ?
C12 Re2 N2 97.0(2) . . ?
C12 Re2 O10 176.02(19) . . ?
C12 Re2 O12 97.48(18) . . ?
N2 Re2 O10 79.54(15) . . ?
O12 Re2 N2 75.28(14) . . ?
O12 Re2 O10 79.84(14) . . ?

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
O4 H4A O12 0.84(8) 1.83(8) 2.656(5) 165(8) 3_667 yes
O4 H4B O11 0.84(8) 1.84(8) 2.667(5) 169(8) 1_656 yes
O10 H10A O5 0.80(8) 1.92(8) 2.687(5) 160(8) . yes
O10 H10B O6 0.84(9) 1.90(9) 2.723(5) 166(8) 3_667 yes
C7 H7 O1 0.95 2.64 3.258(7) 122.8 1_455 yes
C13 H13 O9 0.95 2.53 3.233(6) 131.4 4_576 yes

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
C4 C5 C6 C7 -3.2(9) . . . . ?
C4 C5 C6 F1 177.0(5) . . . . ?
C5 C4 N1 C8 -0.1(8) . . . . ?
C5 C4 N1 Re1 180.0(4) . . . . ?
C5 C6 C7 C8 1.3(8) . . . . ?
C6 C7 C8 C9 -177.5(5) . . . . ?
C6 C7 C8 N1 1.3(8) . . . . ?
C7 C8 C9 O5 4.0(8) . . . . ?
C7 C8 C9 O6 -176.5(5) . . . . ?
C7 C8 N1 C4 -1.9(8) . . . . ?
C7 C8 N1 Re1 178.0(4) . . . . ?
C8 C9 O6 Re1 -3.8(5) . . . . ?
C9 C8 N1 C4 176.9(4) . . . . ?
C9 C8 N1 Re1 -3.1(5) . . . . ?
C13 C14 C15 C16 -0.5(9) . . . . ?
C13 C14 C15 F2 -180.0(5) . . . . ?
C14 C13 N2 C17 -0.2(7) . . . . ?
C14 C13 N2 Re2 -174.0(4) . . . . ?
C14 C15 C16 C17 0.5(9) . . . . ?
C15 C16 C17 C18 -179.1(5) . . . . ?
C15 C16 C17 N2 -0.3(9) . . . . ?
C16 C17 C18 O11 3.6(8) . . . . ?
C16 C17 C18 O12 -177.0(5) . . . . ?
C16 C17 N2 C13 0.2(8) . . . . ?
C16 C17 N2 Re2 174.6(4) . . . . ?
C17 C18 O12 Re2 0.4(6) . . . . ?
C18 C17 N2 C13 179.0(4) . . . . ?
C18 C17 N2 Re2 -6.5(6) . . . . ?
F1 C6 C7 C8 -178.8(5) . . . . ?
F2 C15 C16 C17 180.0(5) . . . . ?
N1 C4 C5 C6 2.6(8) . . . . ?
N1 C8 C9 O5 -174.8(4) . . . . ?
N1 C8 C9 O6 4.6(6) . . . . ?
N2 C13 C14 C15 0.3(8) . . . . ?
N2 C17 C18 O11 -175.3(5) . . . . ?
N2 C17 C18 O12 4.1(7) . . . . ?
O5 C9 O6 Re1 175.5(4) . . . . ?
O11 C18 O12 Re2 179.8(4) . . . . ?


####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2205505'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 Cl N O6 Re'
_chemical_formula_sum            'C9 H5 Cl N O6 Re'
_chemical_formula_weight         444.79
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.25530(10)
_cell_length_b                   7.15140(10)
_cell_length_c                   19.0448(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.8380(10)
_cell_angle_gamma                90
_cell_volume                     1122.97(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10044
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.2700
_cell_measurement_theta_min      4.6200
_shelx_estimated_absorpt_T_max   0.385
_shelx_estimated_absorpt_T_min   0.067
_exptl_absorpt_coefficient_mu    23.598
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.631
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 0 -5 0.0283
-3 0 5 0.0223
1 0 5 0.0777
1 2 2 0.1093
-1 -4 -1 0.0913
0 2 -5 0.1011
5 0 -3 0.0334
-2 0 -5 0.0884
-1 -1 -5 0.0858
-2 0 5 0.0298

_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05

_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.415
_diffrn_reflns_theta_min         4.649
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00  31.00   1.00    1.00    --  -42.36  37.00 -60.00   96
  2  ω     20.00 115.00   1.00    1.00    --   42.36  37.00 120.00   95
  3  ω     27.00  97.00   1.00    1.00    --   42.36-125.00 -90.00   70
  4  ω    -31.00  65.00   1.00    1.00    --   42.36 -37.00  60.00   96
  5  ω     30.00 107.00   1.00    3.00    --  111.00 -94.00 -60.00   77
  6  ω     36.00 109.00   1.00    3.00    --  111.00-111.00 -90.00   73
  7  ω    103.00 178.00   1.00    3.00    --  111.00  77.00 -90.00   75
  8  ω     84.00 178.00   1.00    3.00    --  111.00  57.00  74.18   94
  9  ω    103.00 178.00   1.00    3.00    --  111.00  77.00  30.00   75
 10  ω     36.00 109.00   1.00    3.00    --  111.00-111.00-180.00   73
 11  ω     36.00 109.00   1.00    3.00    --  111.00-111.00 150.00   73
 12  ω     36.00 109.00   1.00    3.00    --  111.00-111.00-150.00   73
 13  ω     36.00 109.00   1.00    3.00    --  111.00-111.00-120.00   73
 14  ω     36.00 109.00   1.00    3.00    --  111.00-111.00 -60.00   73
 15  ω    104.00 178.00   1.00    3.00    --  111.00 111.00-150.00   74
 16  ω     40.00 135.00   1.00    3.00    --  111.00 -45.00 -90.00   95
 17  ω     10.00  42.00   1.00    1.00    --   42.36  79.00-101.84   32
 18  ω     10.00  42.00   1.00    1.00    --   42.36  79.00 -32.09   32
 19  ω     10.00  42.00   1.00    1.00    --   42.36  82.00  25.33   32
 20  ω     12.00 119.00   1.00    1.00    --   42.36  24.00  35.00  107
 21  ω     20.00 115.00   1.00    1.00    --   42.36  37.00-150.00   95
 22  ω     66.00 178.00   1.00    3.00    --  111.00  15.00-150.00  112
 23  ω     87.00 178.00   1.00    3.00    --  111.00  30.00   0.00   91
 24  ω     87.00 118.00   1.00    3.00    --  111.00  30.00 -90.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0925309000
_diffrn_orient_matrix_UB_12      0.1798661000
_diffrn_orient_matrix_UB_13      0.0174644000
_diffrn_orient_matrix_UB_21      0.1479799000
_diffrn_orient_matrix_UB_22      0.1180435000
_diffrn_orient_matrix_UB_23      -0.0186953000
_diffrn_orient_matrix_UB_31      -0.0666804000
_diffrn_orient_matrix_UB_32      0.0120020000
_diffrn_orient_matrix_UB_33      -0.0768249000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2284
_reflns_number_total             2287

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00047(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0193
_refine_ls_restrained_S_all      1.226
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+2.1277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0519
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.4140(4) 0.9248(5) 0.38624(18) 0.0213(7) Uani 1 1 d . . . . .
C2 C 0.7158(4) 1.0181(5) 0.43164(17) 0.0200(6) Uani 1 1 d . . . . .
C3 C 0.5820(4) 0.7184(5) 0.48238(19) 0.0208(7) Uani 1 1 d . . . . .
C4 C 0.9859(5) 0.6873(5) 0.4114(2) 0.0240(8) Uani 1 1 d . . . . .
H4 H 0.994413 0.802690 0.436018 0.029 Uiso 1 1 calc R U . . .
C5 C 1.1229(4) 0.5793(5) 0.4061(2) 0.0249(7) Uani 1 1 d . . . . .
H5 H 1.223122 0.617584 0.428242 0.030 Uiso 1 1 calc R U . . .
C6 C 1.1125(4) 0.4148(5) 0.36828(19) 0.0216(7) Uani 1 1 d . . . . .
H6 H 1.206033 0.339779 0.362749 0.026 Uiso 1 1 calc R U . . .
C7 C 0.9630(4) 0.3609(5) 0.33847(17) 0.0190(6) Uani 1 1 d . . . . .
C8 C 0.8263(4) 0.4718(5) 0.34719(16) 0.0169(6) Uani 1 1 d . . . . .
C9 C 0.6534(4) 0.4286(4) 0.32147(16) 0.0169(6) Uani 1 1 d . . . . .
Cl1 Cl 0.95728(10) 0.15697(13) 0.29029(5) 0.02793(19) Uani 1 1 d . . . . .
N1 N 0.8412(3) 0.6353(4) 0.38309(14) 0.0171(5) Uani 1 1 d . . . . .
O1 O 0.2893(3) 0.9965(4) 0.38340(16) 0.0327(6) Uani 1 1 d . . . . .
O2 O 0.7799(3) 1.1455(4) 0.45798(14) 0.0280(6) Uani 1 1 d . . . . .
O3 O 0.5581(4) 0.6726(4) 0.53881(14) 0.0278(6) Uani 1 1 d . . . . .
O4 O 0.6639(3) 0.8769(3) 0.28074(13) 0.0196(5) Uani 1 1 d D . . . .
H4A H 0.584(4) 0.833(7) 0.259(3) 0.045(16) Uiso 1 1 d D . . . .
H4B H 0.658(7) 0.989(2) 0.273(3) 0.057(18) Uiso 1 1 d D . . . .
O5 O 0.6187(3) 0.2811(3) 0.29000(14) 0.0227(5) Uani 1 1 d . . . . .
O6 O 0.5492(3) 0.5531(3) 0.33493(12) 0.0175(4) Uani 1 1 d . . . . .
Re1 Re 0.62044(2) 0.80030(2) 0.38975(2) 0.01532(8) 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
C1 O1 1.149(4) . ?
C1 Re1 1.921(3) . ?
C2 O2 1.156(4) . ?
C2 Re1 1.902(3) . ?
C3 O3 1.150(5) . ?
C3 Re1 1.900(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.377(5) . ?
C4 N1 1.339(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(5) . ?
C7 C8 1.396(5) . ?
C7 Cl1 1.723(3) . ?
C8 C9 1.518(4) . ?
C8 N1 1.357(4) . ?
C9 O5 1.240(4) . ?
C9 O6 1.273(4) . ?
N1 Re1 2.180(3) . ?
O4 H4A 0.821(10) . ?
O4 H4B 0.818(10) . ?
O4 Re1 2.194(2) . ?
O6 Re1 2.121(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
O1 C1 Re1 178.7(3) . . ?
O2 C2 Re1 176.9(3) . . ?
O3 C3 Re1 178.6(3) . . ?
C5 C4 H4 118.8 . . ?
N1 C4 H4 118.8 . . ?
N1 C4 C5 122.3(3) . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.1(3) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.7(3) . . ?
C7 C6 H6 120.6 . . ?
C6 C7 C8 120.1(3) . . ?
C6 C7 Cl1 116.9(3) . . ?
C8 C7 Cl1 122.9(3) . . ?
C7 C8 C9 126.8(3) . . ?
N1 C8 C7 119.7(3) . . ?
N1 C8 C9 113.5(3) . . ?
O5 C9 C8 121.4(3) . . ?
O5 C9 O6 123.4(3) . . ?
O6 C9 C8 115.3(3) . . ?
C4 N1 C8 119.9(3) . . ?
C4 N1 Re1 123.9(2) . . ?
C8 N1 Re1 116.1(2) . . ?
H4A O4 H4B 104(6) . . ?
Re1 O4 H4A 102(4) . . ?
Re1 O4 H4B 114(4) . . ?
C9 O6 Re1 120.5(2) . . ?
C1 Re1 N1 172.56(12) . . ?
C1 Re1 O4 92.16(12) . . ?
C1 Re1 O6 98.35(12) . . ?
C2 Re1 C1 89.02(14) . . ?
C2 Re1 N1 97.93(12) . . ?
C2 Re1 O4 96.25(12) . . ?
C2 Re1 O6 170.92(12) . . ?
C3 Re1 C1 89.24(15) . . ?
C3 Re1 C2 87.00(14) . . ?
C3 Re1 N1 93.76(13) . . ?
C3 Re1 O4 176.48(12) . . ?
C3 Re1 O6 98.34(12) . . ?
N1 Re1 O4 84.48(10) . . ?
O6 Re1 N1 74.49(9) . . ?
O6 Re1 O4 78.27(9) . . ?

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
O4 H4A O5 0.821(10) 1.914(15) 2.723(4) 169(6) 2_655 yes
O4 H4B O5 0.818(10) 2.14(2) 2.921(3) 160(6) 1_565 yes

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
C4 C5 C6 C7 -1.8(6) . . . . ?
C5 C4 N1 C8 -0.6(6) . . . . ?
C5 C4 N1 Re1 -180.0(3) . . . . ?
C5 C6 C7 C8 -0.3(5) . . . . ?
C5 C6 C7 Cl1 178.7(3) . . . . ?
C6 C7 C8 C9 -176.6(3) . . . . ?
C6 C7 C8 N1 2.0(5) . . . . ?
C7 C8 C9 O5 1.3(5) . . . . ?
C7 C8 C9 O6 -179.0(3) . . . . ?
C7 C8 N1 C4 -1.6(5) . . . . ?
C7 C8 N1 Re1 177.9(2) . . . . ?
C8 C9 O6 Re1 -0.1(4) . . . . ?
C9 C8 N1 C4 177.2(3) . . . . ?
C9 C8 N1 Re1 -3.3(3) . . . . ?
Cl1 C7 C8 C9 4.5(5) . . . . ?
Cl1 C7 C8 N1 -176.9(2) . . . . ?
N1 C4 C5 C6 2.3(6) . . . . ?
N1 C8 C9 O5 -177.4(3) . . . . ?
N1 C8 C9 O6 2.3(4) . . . . ?
O5 C9 O6 Re1 179.6(2) . . . . ?


####################################################################### 
# 
# 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_19
_database_code_depnum_ccdc_archive 'CCDC 2205508'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O7 Re'
_chemical_formula_sum            'C10 H8 N O7 Re'
_chemical_formula_weight         440.37
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.3206(6)
_cell_length_b                   11.8306(2)
_cell_length_c                   9.3609(2)
_cell_angle_alpha                90
_cell_angle_beta                 121.786(3)
_cell_angle_gamma                90
_cell_volume                     2383.57(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9074
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.0630
_cell_measurement_theta_min      4.0700
_shelx_estimated_absorpt_T_max   0.687
_shelx_estimated_absorpt_T_min   0.164
_exptl_absorpt_coefficient_mu    20.274
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-8 -2 5 0.0579
9 0 -5 0.0589
2 -5 -1 0.0530
-2 5 1 0.0530
-1 0 0 0.0105
1 0 0 0.0105

_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02

_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.424
_diffrn_reflns_theta_min         4.108
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -7.00   0.80    5.00    --  -42.36 125.00  60.00  100
  2  ω   -114.00 -58.00   0.80    5.00    --  -42.36-153.00 130.00   70
  3  ω   -113.00 -17.00   0.80    5.00    --  -42.36 -57.00-180.00  120
  4  ω    -87.00  -7.00   0.80    5.00    --  -42.36 125.00   0.00  100
  5  ω    104.00 177.60   0.80   20.00    --  111.00 111.00  60.00   92
  6  ω    103.00 177.40   0.80   20.00    --  111.00  77.00 120.00   93
  7  ω     40.00 134.40   0.80   20.00    --  111.00 -45.00  30.00  118
  8  ω     83.00 177.40   0.80   20.00    --  111.00  61.00  60.00  118
  9  ω     36.00 108.00   0.80   20.00    --  111.00-111.00-120.00   90
 10  ω    103.00 177.40   0.80   20.00    --  111.00  77.00-120.00   93
 11  ω    104.00 177.60   0.80   20.00    --  111.00 111.00   0.00   92
 12  ω    104.00 177.60   0.80   20.00    --  111.00 111.00-150.00   92
 13  ω    103.00 177.40   0.80   20.00    --  111.00  77.00 150.00   93
 14  ω    104.00 177.60   0.80   20.00    --  111.00 111.00 150.00   92
 15  ω    103.00 177.40   0.80   20.00    --  111.00  77.00  90.00   93
 16  ω     36.00 108.00   0.80   20.00    --  111.00-111.00  30.00   90
 17  ω     87.00 177.40   0.80   20.00    --  111.00  30.00-120.00  113
 18  ω   -113.00 -17.00   0.80    5.00    --  -42.36 -57.00 -30.00  120
 19  ω   -113.00 -17.00   0.80    5.00    --  -42.36 -57.00-120.00  120
 20  ω    -69.00  27.00   0.80    5.00    --  -42.36  57.00 -30.00  120
 21  ω   -115.00 -20.60   0.80    5.00    --  -42.36 -37.00  60.00  118
 22  ω     66.00 140.40   0.80   20.00    --  111.00  15.00   0.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0617932000
_diffrn_orient_matrix_UB_12      0.0329475000
_diffrn_orient_matrix_UB_13      -0.1599590000
_diffrn_orient_matrix_UB_21      0.0351972000
_diffrn_orient_matrix_UB_22      0.0800616000
_diffrn_orient_matrix_UB_23      -0.0512674000
_diffrn_orient_matrix_UB_31      0.0080646000
_diffrn_orient_matrix_UB_32      -0.0972978000
_diffrn_orient_matrix_UB_33      -0.0963257000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2387
_reflns_number_total             2434

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.000081(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2434
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0237
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+6.1815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0668
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.67780(18) -0.0620(3) 0.6459(5) 0.0275(7) Uani 1 1 d . . . . .
C2 C 0.71939(18) 0.1205(3) 0.8343(5) 0.0267(7) Uani 1 1 d . . . . .
C3 C 0.7315(2) 0.1110(3) 0.5781(5) 0.0258(8) Uani 1 1 d . . . . .
C4 C 0.64899(17) 0.3653(3) 0.6078(4) 0.0243(6) Uani 1 1 d . . . . .
H4 H 0.677784 0.359351 0.725387 0.029 Uiso 1 1 calc R U . . .
C5 C 0.62895(16) 0.4718(3) 0.5391(4) 0.0259(7) Uani 1 1 d . . . . .
H5 H 0.642702 0.536921 0.608867 0.031 Uiso 1 1 calc R U . . .
C6 C 0.58836(16) 0.4821(3) 0.3663(5) 0.0251(7) Uani 1 1 d . . . . .
C7 C 0.56724(16) 0.3828(3) 0.2700(4) 0.0247(7) Uani 1 1 d . . . . .
H7 H 0.538525 0.386327 0.152125 0.030 Uiso 1 1 calc R U . . .
C8 C 0.58870(15) 0.2806(3) 0.3487(4) 0.0223(6) Uani 1 1 d . . . . .
C9 C 0.56661(15) 0.1723(3) 0.2517(4) 0.0235(6) Uani 1 1 d . . . . .
C10 C 0.5851(2) 0.6829(3) 0.3733(5) 0.0365(9) Uani 1 1 d . . . . .
H10A H 0.569413 0.746798 0.295043 0.055 Uiso 1 1 calc R U . . .
H10B H 0.630509 0.686572 0.442922 0.055 Uiso 1 1 calc R U . . .
H10C H 0.567825 0.686160 0.445557 0.055 Uiso 1 1 calc R U . . .
N1 N 0.62966(13) 0.2697(2) 0.5162(3) 0.0213(5) Uani 1 1 d . . . . .
O1 O 0.68742(14) -0.1565(2) 0.6730(4) 0.0383(6) Uani 1 1 d . . . . .
O2 O 0.75659(13) 0.1322(2) 0.9742(3) 0.0347(6) Uani 1 1 d . . . . .
O3 O 0.77539(14) 0.1206(3) 0.5734(4) 0.0341(6) Uani 1 1 d . . . . .
O4 O 0.58141(14) 0.09101(19) 0.6313(4) 0.0249(6) Uani 1 1 d D . . . .
H4A H 0.5450(8) 0.108(4) 0.566(5) 0.036(14) Uiso 1 1 d D . . . .
H4B H 0.580(3) 0.041(3) 0.690(6) 0.052(15) Uiso 1 1 d D . . . .
O5 O 0.52706(12) 0.1750(2) 0.1007(3) 0.0304(5) Uani 1 1 d . . . . .
O6 O 0.59096(13) 0.0811(2) 0.3367(3) 0.0245(5) Uani 1 1 d . . . . .
O7 O 0.56667(15) 0.5787(2) 0.2801(4) 0.0327(6) Uani 1 1 d . . . . .
Re1 Re 0.66118(2) 0.09668(2) 0.60113(2) 0.02055(10) 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
C1 O1 1.144(5) . ?
C1 Re1 1.922(4) . ?
C2 O2 1.149(5) . ?
C2 Re1 1.905(4) . ?
C3 O3 1.140(5) . ?
C3 Re1 1.911(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(5) . ?
C4 N1 1.346(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(5) . ?
C6 C7 1.404(5) . ?
C6 O7 1.339(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.369(5) . ?
C8 C9 1.499(4) . ?
C8 N1 1.356(4) . ?
C9 O5 1.229(4) . ?
C9 O6 1.289(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 O7 1.439(5) . ?
N1 Re1 2.188(3) . ?
O4 H4A 0.818(10) . ?
O4 H4B 0.820(10) . ?
O4 Re1 2.183(3) . ?
O6 Re1 2.165(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 179.5(3) . . ?
O2 C2 Re1 176.7(3) . . ?
O3 C3 Re1 176.4(4) . . ?
C5 C4 H4 118.4 . . ?
N1 C4 H4 118.4 . . ?
N1 C4 C5 123.2(3) . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.1(3) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C7 118.1(3) . . ?
O7 C6 C5 126.4(3) . . ?
O7 C6 C7 115.5(3) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 118.9(3) . . ?
C8 C7 H7 120.5 . . ?
C7 C8 C9 120.9(3) . . ?
N1 C8 C7 123.5(3) . . ?
N1 C8 C9 115.6(3) . . ?
O5 C9 C8 119.5(3) . . ?
O5 C9 O6 124.5(3) . . ?
O6 C9 C8 115.9(3) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C10 H10A 109.5 . . ?
O7 C10 H10B 109.5 . . ?
O7 C10 H10C 109.5 . . ?
C4 N1 C8 117.1(3) . . ?
C4 N1 Re1 127.9(2) . . ?
C8 N1 Re1 114.8(2) . . ?
H4A O4 H4B 104(5) . . ?
Re1 O4 H4A 131(4) . . ?
Re1 O4 H4B 119(4) . . ?
C9 O6 Re1 118.2(2) . . ?
C6 O7 C10 117.8(3) . . ?
C1 Re1 N1 171.54(13) . . ?
C1 Re1 O4 93.03(12) . . ?
C1 Re1 O6 96.87(13) . . ?
C2 Re1 C1 86.91(16) . . ?
C2 Re1 C3 84.92(17) . . ?
C2 Re1 N1 101.07(14) . . ?
C2 Re1 O4 93.80(14) . . ?
C2 Re1 O6 175.44(12) . . ?
C3 Re1 C1 90.07(16) . . ?
C3 Re1 N1 93.40(13) . . ?
C3 Re1 O4 176.58(12) . . ?
C3 Re1 O6 97.57(15) . . ?
O4 Re1 N1 83.71(9) . . ?
O6 Re1 N1 75.03(10) . . ?
O6 Re1 O4 83.49(11) . . ?

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
C4 C5 C6 C7 2.9(5) . . . . ?
C4 C5 C6 O7 -177.3(3) . . . . ?
C5 C4 N1 C8 0.2(5) . . . . ?
C5 C4 N1 Re1 175.5(3) . . . . ?
C5 C6 C7 C8 -1.9(5) . . . . ?
C5 C6 O7 C10 -2.0(6) . . . . ?
C6 C7 C8 C9 178.9(3) . . . . ?
C6 C7 C8 N1 0.0(5) . . . . ?
C7 C6 O7 C10 177.8(3) . . . . ?
C7 C8 C9 O5 -2.6(5) . . . . ?
C7 C8 C9 O6 178.1(3) . . . . ?
C7 C8 N1 C4 0.9(5) . . . . ?
C7 C8 N1 Re1 -175.0(3) . . . . ?
C8 C9 O6 Re1 -1.9(4) . . . . ?
C9 C8 N1 C4 -178.0(3) . . . . ?
C9 C8 N1 Re1 6.1(4) . . . . ?
N1 C4 C5 C6 -2.1(5) . . . . ?
N1 C8 C9 O5 176.3(3) . . . . ?
N1 C8 C9 O6 -2.9(4) . . . . ?
O5 C9 O6 Re1 178.9(3) . . . . ?
O7 C6 C7 C8 178.3(3) . . . . ?

####################################################################### 
# 
# 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_15
_database_code_depnum_ccdc_archive 'CCDC 2205509'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-05-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O6 Re'
_chemical_formula_sum            'C10 H8 N O6 Re'
_chemical_formula_weight         424.37
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   9.2924(2)
_cell_length_b                   11.1464(3)
_cell_length_c                   22.2675(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.090(2)
_cell_angle_gamma                90
_cell_volume                     2270.72(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7026
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.6210
_cell_measurement_theta_min      4.0340
_shelx_estimated_absorpt_T_max   0.417
_shelx_estimated_absorpt_T_min   0.101
_exptl_absorpt_coefficient_mu    21.174
_exptl_absorpt_correction_T_max  0.423
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 5 0.0175
1 0 -5 0.0365
-1 -1 -1 0.0939
1 1 1 0.0939
-4 5 0 0.0545
0 0 1 0.0282
5 -4 2 0.0668
-2 -1 -5 0.0744
1 -3 -5 0.0611
2 -5 2 0.0481
1 0 5 0.0558
-1 0 -5 0.0623

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05

_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10677
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.397
_diffrn_reflns_theta_min         4.033
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00 124.00   0.50    0.10    --   51.04  76.00  31.00  190
  2  ω     86.00 178.00   0.50    0.21    --  107.75  76.00  31.00  184
  3  ω     96.00 176.00   0.50    0.21    --  107.75  30.00 120.00  160
  4  ω    146.00 174.00   0.50    0.21    --  107.75  45.00-120.00   56
  5  ω    139.00 176.00   0.50    0.21    --  107.75  15.00-180.00   74
  6  ω     96.00 135.00   0.50    0.21    --  107.75  15.00-180.00   78
  7  ω     42.00  69.00   0.50    0.21    --  107.75 -94.00   0.00   54
  8  ω     46.00  91.00   0.50    0.21    --  107.75-111.00  90.00   90
  9  ω     65.00  92.00   0.50    0.21    --  107.75-111.00 120.00   54
 10  ω     36.00 101.00   0.50    0.21    --  107.75 -94.00  90.00  130
 11  ω     32.00 104.00   0.50    0.21    --  107.75 -94.00 -90.00  144
 12  ω     32.00  69.00   0.50    0.21    --  107.75 -94.00-180.00   74
 13  ω     29.00  58.00   0.50    0.21    --  107.75 -15.00-120.00   58
 14  ω    -22.00  73.00   0.50    0.10    --   51.04 -76.00 -94.00  190
 15  ω     35.00 130.00   0.50    0.21    --  107.75 -76.00 -94.00  190
 16  ω     34.00 120.00   0.50    0.21    --  107.75 -30.00 -90.00  172
 17  ω     74.00 115.00   0.50    0.21    --  107.75 -15.00-120.00   82
 18  ω    118.00 178.00   0.50    0.21    --  107.75 111.00-120.00  120
 19  ω    104.00 145.00   0.50    0.21    --  107.75 178.00 -90.00   82
 20  ω    -73.00  22.00   0.50    0.10    --  -51.04  76.00  31.00  190
 21  ω    -83.00 -12.00   0.50    0.10    --  -51.04 125.00 120.00  142
 22  ω   -108.00 -13.00   0.50    0.21    --  -86.25  76.00  31.00  190
 23  ω   -126.00 -73.00   0.50    0.10    --  -51.04-125.00   0.00  106
 24  ω   -126.00 -73.00   0.50    0.10    --  -51.04-125.00 -60.00  106
 25  ω   -126.00 -73.00   0.50    0.10    --  -51.04-125.00-180.00  106
 26  ω   -159.00 -64.00   0.50    0.21    --  -86.25 -76.00 -94.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1379261000
_diffrn_orient_matrix_UB_12      -0.0018989000
_diffrn_orient_matrix_UB_13      -0.0497794000
_diffrn_orient_matrix_UB_21      -0.0582191000
_diffrn_orient_matrix_UB_22      -0.1089874000
_diffrn_orient_matrix_UB_23      0.0310176000
_diffrn_orient_matrix_UB_31      -0.0772282000
_diffrn_orient_matrix_UB_32      0.0850608000
_diffrn_orient_matrix_UB_33      0.0386779000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2223
_reflns_number_total             2298

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.000040(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0246
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0338P)²+16.7274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.4530(5) 0.5722(5) 0.6691(2) 0.0273(10) Uani 1 1 d . . . . .
C2 C 0.6028(5) 0.3811(4) 0.7147(2) 0.0245(9) Uani 1 1 d . . . . .
C3 C 0.3325(5) 0.3897(4) 0.7240(2) 0.0214(9) Uani 1 1 d . . . . .
C4 C 0.4657(5) 0.1187(4) 0.6554(2) 0.0239(9) Uani 1 1 d . . . . .
H4 H 0.551460 0.131772 0.684844 0.029 Uiso 1 1 calc R U . . .
C5 C 0.4261(5) 0.0036(4) 0.6392(2) 0.0243(9) Uani 1 1 d . . . . .
H5 H 0.485309 -0.061131 0.656926 0.029 Uiso 1 1 calc R U . . .
C6 C 0.2988(5) -0.0204(4) 0.5967(2) 0.0244(9) Uani 1 1 d . . . . .
C7 C 0.2187(5) 0.0789(4) 0.5719(2) 0.0239(9) Uani 1 1 d . . . . .
H7 H 0.131765 0.068137 0.542885 0.029 Uiso 1 1 calc R U . . .
C8 C 0.2660(5) 0.1933(4) 0.58962(19) 0.0222(8) Uani 1 1 d . . . . .
C9 C 0.1841(5) 0.3032(4) 0.56334(19) 0.0228(8) Uani 1 1 d . . . . .
C10 C 0.2523(6) -0.1466(4) 0.5799(2) 0.0301(10) Uani 1 1 d . . . . .
H10A H 0.327033 -0.185991 0.560730 0.045 Uiso 1 1 calc R U . . .
H10B H 0.159341 -0.145501 0.551218 0.045 Uiso 1 1 calc R U . . .
H10C H 0.240117 -0.190822 0.616697 0.045 Uiso 1 1 calc R U . . .
N1 N 0.3874(4) 0.2150(3) 0.63107(16) 0.0211(7) Uani 1 1 d . . . . .
O1 O 0.4693(4) 0.6725(3) 0.67729(18) 0.0371(8) Uani 1 1 d . . . . .
O2 O 0.7037(4) 0.3679(3) 0.75191(16) 0.0296(7) Uani 1 1 d . . . . .
O3 O 0.2791(4) 0.3795(3) 0.76626(16) 0.0303(7) Uani 1 1 d . . . . .
O4 O 0.5439(4) 0.4059(3) 0.57776(17) 0.0288(8) Uani 1 1 d . . . . .
H4A H 0.506(7) 0.382(5) 0.548(3) 0.028(16) Uiso 1 1 d . . . . .
H4B H 0.590(7) 0.461(6) 0.570(3) 0.035(17) Uiso 1 1 d . . . . .
O5 O 0.0751(4) 0.2922(3) 0.52373(15) 0.0299(7) Uani 1 1 d . . . . .
O6 O 0.2363(4) 0.4048(3) 0.58531(15) 0.0247(7) Uani 1 1 d . . . . .
Re1 Re 0.42964(2) 0.40173(2) 0.65575(2) 0.02019(10) 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
C1 O1 1.138(6) . ?
C1 Re1 1.930(5) . ?
C2 O2 1.147(6) . ?
C2 Re1 1.904(5) . ?
C3 O3 1.144(6) . ?
C3 Re1 1.903(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(7) . ?
C4 N1 1.355(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.405(6) . ?
C6 C7 1.393(7) . ?
C6 C10 1.500(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(6) . ?
C8 C9 1.505(6) . ?
C8 N1 1.349(6) . ?
C9 O5 1.227(5) . ?
C9 O6 1.294(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N1 Re1 2.171(4) . ?
O4 H4A 0.74(7) . ?
O4 H4B 0.78(7) . ?
O4 Re1 2.189(4) . ?
O6 Re1 2.168(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 178.8(4) . . ?
O2 C2 Re1 177.2(4) . . ?
O3 C3 Re1 177.0(4) . . ?
C5 C4 H4 118.8 . . ?
N1 C4 H4 118.8 . . ?
N1 C4 C5 122.5(4) . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.9(4) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C10 121.2(4) . . ?
C7 C6 C5 116.4(4) . . ?
C7 C6 C10 122.4(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 121.7(4) . . ?
N1 C8 C7 123.1(4) . . ?
N1 C8 C9 115.2(4) . . ?
O5 C9 C8 119.7(4) . . ?
O5 C9 O6 124.5(4) . . ?
O6 C9 C8 115.8(4) . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 N1 Re1 126.7(3) . . ?
C8 N1 C4 117.3(4) . . ?
C8 N1 Re1 116.0(3) . . ?
H4A O4 H4B 106(6) . . ?
Re1 O4 H4A 118(5) . . ?
Re1 O4 H4B 124(5) . . ?
C9 O6 Re1 117.9(3) . . ?
C1 Re1 N1 173.54(17) . . ?
C1 Re1 O4 92.55(17) . . ?
C1 Re1 O6 98.79(16) . . ?
C2 Re1 C1 87.3(2) . . ?
C2 Re1 N1 98.76(16) . . ?
C2 Re1 O4 94.61(17) . . ?
C2 Re1 O6 173.55(16) . . ?
C3 Re1 C1 90.13(19) . . ?
C3 Re1 C2 84.45(19) . . ?
C3 Re1 N1 92.55(16) . . ?
C3 Re1 O4 177.12(16) . . ?
C3 Re1 O6 97.47(16) . . ?
N1 Re1 O4 84.89(14) . . ?
O6 Re1 N1 75.04(12) . . ?
O6 Re1 O4 83.18(14) . . ?

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
O4 H4A O5 0.74(7) 1.92(7) 2.657(5) 169(7) 2_556 yes
O4 H4B O6 0.78(7) 2.01(7) 2.752(5) 157(6) 6_665 yes

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
C4 C5 C6 C7 1.0(6) . . . . ?
C4 C5 C6 C10 -178.3(4) . . . . ?
C5 C4 N1 C8 0.3(6) . . . . ?
C5 C4 N1 Re1 176.4(3) . . . . ?
C5 C6 C7 C8 -0.1(6) . . . . ?
C6 C7 C8 C9 179.0(4) . . . . ?
C6 C7 C8 N1 -0.8(7) . . . . ?
C7 C8 C9 O5 -2.3(6) . . . . ?
C7 C8 C9 O6 177.5(4) . . . . ?
C7 C8 N1 C4 0.7(6) . . . . ?
C7 C8 N1 Re1 -175.8(3) . . . . ?
C8 C9 O6 Re1 -0.3(5) . . . . ?
C9 C8 N1 C4 -179.2(4) . . . . ?
C9 C8 N1 Re1 4.3(5) . . . . ?
C10 C6 C7 C8 179.2(4) . . . . ?
N1 C4 C5 C6 -1.1(7) . . . . ?
N1 C8 C9 O5 177.5(4) . . . . ?
N1 C8 C9 O6 -2.7(5) . . . . ?
O5 C9 O6 Re1 179.5(3) . . . . ?

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2205511'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C10 H8 N O6 Re), H2 O'
_chemical_formula_sum            'C20 H18 N2 O13 Re2'
_chemical_formula_weight         866.76
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   22.7527(2)
_cell_length_b                   10.61400(10)
_cell_length_c                   21.7337(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.9160(10)
_cell_angle_gamma                90
_cell_volume                     4934.72(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16471
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.0220
_cell_measurement_theta_min      3.4290
_shelx_estimated_absorpt_T_max   0.592
_shelx_estimated_absorpt_T_min   0.158
_exptl_absorpt_coefficient_mu    19.536
_exptl_absorpt_correction_T_max  0.553
_exptl_absorpt_correction_T_min  0.143
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0500
0 0 1 0.0580
-2 -5 0 0.0234
2 5 0 0.0114
1 0 0 0.0439
-1 0 0 0.0509

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03

_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25330
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.482
_diffrn_reflns_theta_min         4.133
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -20.00   1.00    1.00    --  -42.61 -37.00 -90.00   96
  2  ω    -74.00  31.00   1.00    1.00    --  -42.61  77.00  30.00  105
  3  ω    -30.00  65.00   1.00    1.00    --   42.61 -37.00 -60.00   95
  4  ω     10.00  42.00   1.00    1.00    --   42.61  81.00 -82.38   32
  5  ω     36.00 109.00   1.00    4.00    --  111.00-111.00 -30.00   73
  6  ω     36.00 109.00   1.00    4.00    --  111.00-111.00 120.00   73
  7  ω     40.00 135.00   1.00    4.00    --  111.00 -45.00-120.00   95
  8  ω     83.00 178.00   1.00    4.00    --  111.00  61.00  30.00   95
  9  ω     36.00 109.00   1.00    4.00    --  111.00-111.00  90.00   73
 10  ω     36.00 109.00   1.00    4.00    --  111.00-111.00  30.00   73
 11  ω     38.00 110.00   1.00    4.00    --  111.00-119.00 -48.00   72
 12  ω     36.00 109.00   1.00    4.00    --  111.00-111.00  60.00   73
 13  ω    103.00 178.00   1.00    4.00    --  111.00  77.00 -30.00   75
 14  ω     36.00 109.00   1.00    4.00    --  111.00-111.00   0.00   73
 15  ω    103.00 178.00   1.00    4.00    --  111.00  77.00-120.00   75
 16  ω    104.00 178.00   1.00    4.00    --  111.00 111.00 -30.00   74
 17  ω    103.00 178.00   1.00    4.00    --  111.00  77.00   0.00   75
 18  ω   -121.00  -6.00   1.00    1.00    --  -42.61 -19.00   0.00  115
 19  ω     10.00  42.00   1.00    1.00    --   42.61  81.00  94.37   32
 20  ω     10.00  42.00   1.00    1.00    --   42.61  82.00 163.19   32
 21  ω     82.00 178.00   1.00    4.00    --  111.00  69.00 -68.23   96
 22  ω     66.00 178.00   1.00    4.00    --  111.00  15.00-150.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0047545000
_diffrn_orient_matrix_UB_12      0.1431556000
_diffrn_orient_matrix_UB_13      -0.0125723000
_diffrn_orient_matrix_UB_21      0.0337551000
_diffrn_orient_matrix_UB_22      -0.0153041000
_diffrn_orient_matrix_UB_23      -0.0501568000
_diffrn_orient_matrix_UB_31      -0.0634029000
_diffrn_orient_matrix_UB_32      -0.0188824000
_diffrn_orient_matrix_UB_33      -0.0548973000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4989
_reflns_number_total             5046

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.000036(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0179
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+12.6205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0431
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.20933(17) 0.2896(3) 0.41160(16) 0.0398(7) Uani 1 1 d . . . . .
C2 C 0.28422(16) 0.3241(4) 0.34109(17) 0.0448(9) Uani 1 1 d . . . . .
C3 C 0.17184(14) 0.4293(3) 0.30209(15) 0.0311(6) Uani 1 1 d . . . . .
C4 C 0.30940(15) 0.6433(4) 0.32611(16) 0.0402(8) Uani 1 1 d . . . . .
H4 H 0.328728 0.574146 0.312782 0.048 Uiso 1 1 calc R U . . .
C5 C 0.32243(16) 0.7639(4) 0.31099(16) 0.0479(10) Uani 1 1 d . . . . .
H5 H 0.350589 0.777535 0.287899 0.057 Uiso 1 1 calc R U . . .
C6 C 0.29433(16) 0.8636(4) 0.32965(16) 0.0436(8) Uani 1 1 d . . . . .
H6 H 0.302678 0.946750 0.318656 0.052 Uiso 1 1 calc R U . . .
C7 C 0.25358(14) 0.8456(3) 0.36458(15) 0.0341(7) Uani 1 1 d . . . . .
C8 C 0.24422(12) 0.7202(3) 0.37958(13) 0.0250(5) Uani 1 1 d . . . . .
C9 C 0.20486(12) 0.6834(3) 0.42013(13) 0.0237(5) Uani 1 1 d . . . . .
C10 C 0.22308(17) 0.9560(3) 0.3832(2) 0.0449(8) Uani 1 1 d . . . . .
H10A H 0.177573 0.946496 0.364753 0.067 Uiso 1 1 calc R U . . .
H10B H 0.235548 1.033169 0.366087 0.067 Uiso 1 1 calc R U . . .
H10C H 0.236030 0.961268 0.430979 0.067 Uiso 1 1 calc R U . . .
C11 C 0.52653(17) 0.5067(3) 0.34310(18) 0.0408(8) Uani 1 1 d . . . . .
C12 C 0.56021(15) 0.2845(3) 0.30797(16) 0.0376(7) Uani 1 1 d . . . . .
C13 C 0.44056(16) 0.3501(3) 0.26714(17) 0.0359(7) Uani 1 1 d . . . . .
C14 C 0.49497(14) 0.0401(3) 0.35256(15) 0.0323(6) Uani 1 1 d . . . . .
H14 H 0.517801 0.043028 0.323233 0.039 Uiso 1 1 calc R U . . .
C15 C 0.47995(16) -0.0757(3) 0.37272(18) 0.0403(8) Uani 1 1 d . . . . .
H15 H 0.493508 -0.151565 0.358539 0.048 Uiso 1 1 calc R U . . .
C16 C 0.44519(16) -0.0795(3) 0.41352(17) 0.0375(7) Uani 1 1 d . . . . .
H16 H 0.434020 -0.158621 0.426758 0.045 Uiso 1 1 calc R U . . .
C17 C 0.42608(13) 0.0314(3) 0.43575(15) 0.0297(6) Uani 1 1 d . . . . .
C18 C 0.44474(12) 0.1440(2) 0.41506(13) 0.0230(5) Uani 1 1 d . . . . .
C19 C 0.43100(11) 0.2725(3) 0.43651(13) 0.0231(5) Uani 1 1 d . . . . .
C20 C 0.38640(15) 0.0240(3) 0.47849(17) 0.0389(7) Uani 1 1 d . . . . .
H20A H 0.409434 0.059474 0.521618 0.058 Uiso 1 1 calc R U . . .
H20B H 0.376088 -0.064239 0.483374 0.058 Uiso 1 1 calc R U . . .
H20C H 0.347789 0.071950 0.458364 0.058 Uiso 1 1 calc R U . . .
N1 N 0.27021(10) 0.6207(3) 0.35909(11) 0.0278(5) Uani 1 1 d . . . . .
N2 N 0.47784(11) 0.1478(2) 0.37372(11) 0.0242(5) Uani 1 1 d . . . . .
O1 O 0.18737(16) 0.2087(3) 0.43152(15) 0.0586(8) Uani 1 1 d . . . . .
O2 O 0.30960(13) 0.2567(3) 0.31709(15) 0.0664(10) Uani 1 1 d . . . . .
O3 O 0.13048(11) 0.4301(2) 0.25426(11) 0.0403(5) Uani 1 1 d . . . . .
O4 O 0.32377(10) 0.4659(2) 0.46881(11) 0.0333(5) Uani 1 1 d . . . . .
H4A H 0.349(2) 0.418(5) 0.476(2) 0.054(14) Uiso 1 1 d . . . . .
H4B H 0.318(2) 0.493(5) 0.501(2) 0.050(13) Uiso 1 1 d . . . . .
O5 O 0.20105(9) 0.56414(18) 0.42920(9) 0.0250(4) Uani 1 1 d . . . . .
O6 O 0.17925(9) 0.76280(19) 0.44348(11) 0.0299(4) Uani 1 1 d . . . . .
O7 O 0.53854(17) 0.6101(3) 0.33875(18) 0.0652(9) Uani 1 1 d . . . . .
O8 O 0.59362(13) 0.2503(3) 0.28187(13) 0.0562(7) Uani 1 1 d . . . . .
O9 O 0.40349(14) 0.3633(3) 0.21693(13) 0.0552(7) Uani 1 1 d . . . . .
O10 O 0.57047(10) 0.3079(2) 0.44960(11) 0.0340(5) Uani 1 1 d . . . . .
H10D H 0.568(2) 0.338(4) 0.485(2) 0.044(11) Uiso 1 1 d . . . . .
H10E H 0.603(2) 0.295(5) 0.449(2) 0.053(13) Uiso 1 1 d . . . . .
O11 O 0.44530(9) 0.36653(18) 0.40731(10) 0.0254(4) Uani 1 1 d . . . . .
O12 O 0.40898(10) 0.2845(2) 0.48074(11) 0.0316(4) Uani 1 1 d . . . . .
O13 O 0.54451(10) 0.38651(19) 0.55411(11) 0.0305(4) Uani 1 1 d G . . . .
H13A H 0.550336 0.463629 0.565105 0.046 Uiso 1 1 d G U . . .
H13B H 0.507565 0.365333 0.550907 0.046 Uiso 1 1 d G U . . .
Re1 Re 0.24188(2) 0.43469(2) 0.38104(2) 0.02724(5) Uani 1 1 d . . . . .
Re2 Re 0.50426(2) 0.33433(2) 0.35113(2) 0.02506(5) 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
C1 O1 1.149(5) . ?
C1 Re1 1.923(4) . ?
C2 O2 1.150(4) . ?
C2 Re1 1.905(4) . ?
C3 O3 1.140(4) . ?
C3 Re1 1.904(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.379(6) . ?
C4 N1 1.342(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.368(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.397(5) . ?
C7 C8 1.404(4) . ?
C7 C10 1.487(5) . ?
C8 C9 1.506(4) . ?
C8 N1 1.358(4) . ?
C9 O5 1.289(3) . ?
C9 O6 1.228(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O7 1.142(5) . ?
C11 Re2 1.922(3) . ?
C12 O8 1.151(4) . ?
C12 Re2 1.896(3) . ?
C13 O9 1.138(4) . ?
C13 Re2 1.913(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(5) . ?
C14 N2 1.339(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.375(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.397(5) . ?
C17 C18 1.394(4) . ?
C17 C20 1.502(5) . ?
C18 C19 1.509(4) . ?
C18 N2 1.355(4) . ?
C19 O11 1.282(3) . ?
C19 O12 1.233(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N1 Re1 2.179(3) . ?
N2 Re2 2.173(2) . ?
O4 H4A 0.74(5) . ?
O4 H4B 0.81(5) . ?
O4 Re1 2.191(2) . ?
O5 Re1 2.1235(19) . ?
O10 H10D 0.85(5) . ?
O10 H10E 0.76(5) . ?
O10 Re2 2.175(2) . ?
O11 Re2 2.1267(19) . ?
O13 H13A 0.8504 . ?
O13 H13B 0.8498 . ?

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
O1 C1 Re1 175.1(3) . . ?
O2 C2 Re1 179.5(5) . . ?
O3 C3 Re1 177.6(3) . . ?
C5 C4 H4 119.0 . . ?
N1 C4 H4 119.0 . . ?
N1 C4 C5 122.0(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 H6 119.4 . . ?
C5 C6 C7 121.3(4) . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C8 115.9(3) . . ?
C6 C7 C10 119.8(3) . . ?
C8 C7 C10 124.2(3) . . ?
C7 C8 C9 123.3(3) . . ?
N1 C8 C7 123.0(3) . . ?
N1 C8 C9 113.8(3) . . ?
O5 C9 C8 115.4(2) . . ?
O6 C9 C8 121.6(3) . . ?
O6 C9 O5 123.0(3) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C11 Re2 178.3(3) . . ?
O8 C12 Re2 177.8(3) . . ?
O9 C13 Re2 177.7(3) . . ?
C15 C14 H14 119.4 . . ?
N2 C14 H14 119.4 . . ?
N2 C14 C15 121.1(3) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 120.9(3) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 C20 119.6(3) . . ?
C18 C17 C16 116.5(3) . . ?
C18 C17 C20 123.9(3) . . ?
C17 C18 C19 123.9(3) . . ?
N2 C18 C17 122.6(3) . . ?
N2 C18 C19 113.5(2) . . ?
O11 C19 C18 115.9(2) . . ?
O12 C19 C18 121.1(3) . . ?
O12 C19 O11 123.0(3) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C4 N1 C8 118.6(3) . . ?
C4 N1 Re1 125.4(2) . . ?
C8 N1 Re1 116.00(18) . . ?
C14 N2 C18 119.6(3) . . ?
C14 N2 Re2 124.4(2) . . ?
C18 N2 Re2 115.85(18) . . ?
H4A O4 H4B 114(5) . . ?
Re1 O4 H4A 117(4) . . ?
Re1 O4 H4B 117(3) . . ?
C9 O5 Re1 119.78(18) . . ?
H10D O10 H10E 116(5) . . ?
Re2 O10 H10D 127(3) . . ?
Re2 O10 H10E 112(4) . . ?
C19 O11 Re2 118.37(17) . . ?
H13A O13 H13B 109.4 . . ?
C1 Re1 N1 168.14(12) . . ?
C1 Re1 O4 97.68(12) . . ?
C1 Re1 O5 93.63(11) . . ?
C2 Re1 C1 88.74(17) . . ?
C2 Re1 N1 103.00(15) . . ?
C2 Re1 O4 94.46(11) . . ?
C2 Re1 O5 175.83(12) . . ?
C3 Re1 C1 89.12(14) . . ?
C3 Re1 C2 88.21(13) . . ?
C3 Re1 N1 92.82(11) . . ?
C3 Re1 O4 172.74(12) . . ?
C3 Re1 O5 95.24(10) . . ?
N1 Re1 O4 80.00(9) . . ?
O5 Re1 N1 74.55(8) . . ?
O5 Re1 O4 81.84(8) . . ?
C11 Re2 N2 171.64(12) . . ?
C11 Re2 O10 95.54(13) . . ?
C11 Re2 O11 97.85(11) . . ?
C12 Re2 C11 88.76(15) . . ?
C12 Re2 C13 88.30(14) . . ?
C12 Re2 N2 98.14(13) . . ?
C12 Re2 O10 95.40(12) . . ?
C12 Re2 O11 171.94(12) . . ?
C13 Re2 C11 88.14(15) . . ?
C13 Re2 N2 96.74(12) . . ?
C13 Re2 O10 174.83(12) . . ?
C13 Re2 O11 96.48(12) . . ?
N2 Re2 O10 79.18(9) . . ?
O11 Re2 N2 74.91(8) . . ?
O11 Re2 O10 79.44(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
C5 H5 O8 0.95 2.30 3.220(4) 161.9 4 yes
O4 H4A O12 0.74(5) 1.95(5) 2.681(3) 171(5) . yes
O4 H4B O5 0.81(5) 1.87(5) 2.678(3) 175(5) 2_556 yes
O10 H10D O13 0.85(5) 1.83(5) 2.668(3) 166(4) . yes
O10 H10E O6 0.76(5) 1.88(5) 2.633(3) 171(5) 6_665 yes
O13 H13A O11 0.85 1.89 2.738(3) 173.1 5_666 yes
O13 H13B O12 0.85 2.40 3.142(3) 146.2 . yes

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
C4 C5 C6 C7 1.1(5) . . . . ?
C5 C4 N1 C8 -1.9(4) . . . . ?
C5 C4 N1 Re1 176.3(2) . . . . ?
C5 C6 C7 C8 0.7(5) . . . . ?
C5 C6 C7 C10 -179.1(3) . . . . ?
C6 C7 C8 C9 176.4(3) . . . . ?
C6 C7 C8 N1 -3.2(4) . . . . ?
C7 C8 C9 O5 179.9(3) . . . . ?
C7 C8 C9 O6 -1.2(4) . . . . ?
C7 C8 N1 C4 3.8(4) . . . . ?
C7 C8 N1 Re1 -174.6(2) . . . . ?
C8 C9 O5 Re1 -5.4(3) . . . . ?
C9 C8 N1 C4 -175.8(2) . . . . ?
C9 C8 N1 Re1 5.8(3) . . . . ?
C10 C7 C8 C9 -3.8(5) . . . . ?
C10 C7 C8 N1 176.5(3) . . . . ?
C14 C15 C16 C17 -1.3(5) . . . . ?
C15 C14 N2 C18 -0.6(4) . . . . ?
C15 C14 N2 Re2 175.4(2) . . . . ?
C15 C16 C17 C18 -0.8(4) . . . . ?
C15 C16 C17 C20 178.0(3) . . . . ?
C16 C17 C18 C19 -177.1(3) . . . . ?
C16 C17 C18 N2 2.2(4) . . . . ?
C17 C18 C19 O11 -172.5(2) . . . . ?
C17 C18 C19 O12 9.5(4) . . . . ?
C17 C18 N2 C14 -1.6(4) . . . . ?
C17 C18 N2 Re2 -178.0(2) . . . . ?
C18 C19 O11 Re2 -14.1(3) . . . . ?
C19 C18 N2 C14 177.9(2) . . . . ?
C19 C18 N2 Re2 1.5(3) . . . . ?
C20 C17 C18 C19 4.1(4) . . . . ?
C20 C17 C18 N2 -176.5(3) . . . . ?
N1 C4 C5 C6 -0.5(5) . . . . ?
N1 C8 C9 O5 -0.5(3) . . . . ?
N1 C8 C9 O6 178.4(2) . . . . ?
N2 C14 C15 C16 2.1(5) . . . . ?
N2 C18 C19 O11 8.1(3) . . . . ?
N2 C18 C19 O12 -170.0(2) . . . . ?
O6 C9 O5 Re1 175.7(2) . . . . ?
O12 C19 O11 Re2 163.9(2) . . . . ?


####################################################################### 
# 
# 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_25
_database_code_depnum_ccdc_archive 'CCDC 2205512'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O6 Re, H2 O'
_chemical_formula_sum            'C10 H10 N O7 Re'
_chemical_formula_weight         442.39
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.6859(3)
_cell_length_b                   11.41920(10)
_cell_length_c                   9.1451(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.3100(10)
_cell_angle_gamma                90
_cell_volume                     2556.99(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10069
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1830
_cell_measurement_theta_min      3.5770
_shelx_estimated_absorpt_T_max   0.397
_shelx_estimated_absorpt_T_min   0.084
_exptl_absorpt_coefficient_mu    18.899
_exptl_absorpt_correction_T_max  0.382
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0241
-1 0 0 0.0401
-1 -1 -1 0.0915
2 5 -5 0.1117
-2 -5 5 0.0917
-4 5 4 0.1254
1 -5 -1 0.1299
-5 5 1 0.1402

_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06

_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12718
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.500
_diffrn_reflns_theta_min         3.610
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -16.00   0.50    0.50    --  -42.49 -57.00-120.00  194
  2  ω    -87.00  -6.00   0.50    0.50    --  -42.49 125.00-180.00  162
  3  ω     27.00  98.00   0.50    0.50    --   42.49-125.00 -60.00  142
  4  ω     27.00  98.00   0.50    0.50    --   42.49-125.00  90.00  142
  5  ω    -21.00  74.00   0.50    0.50    --   42.49 -77.00   0.00  190
  6  ω     36.00 109.00   0.50    1.50    --  111.00-111.00  90.00  146
  7  ω     41.00 139.00   0.50    1.50    --  111.00 -61.00  90.00  196
  8  ω     30.00 107.00   0.50    1.50    --  111.00 -94.00 -30.00  154
  9  ω    103.00 178.00   0.50    1.50    --  111.00  77.00-180.00  150
 10  ω    103.00 178.00   0.50    1.50    --  111.00  77.00 120.00  150
 11  ω    103.00 178.00   0.50    1.50    --  111.00  77.00  60.00  150
 12  ω     61.00 146.00   0.50    1.50    --  111.00 178.00-150.00  170
 13  ω     87.00 178.00   0.50    1.50    --  111.00  45.00 120.00  182
 14  ω     36.00 109.00   0.50    1.50    --  111.00-111.00-180.00  146
 15  ω    104.00 178.00   0.50    1.50    --  111.00 111.00 120.00  148
 16  ω     61.00 146.00   0.50    1.50    --  111.00 178.00 -30.00  170
 17  ω   -113.00 -16.00   0.50    0.50    --  -42.49 -57.00 120.00  194
 18  ω   -113.00 -16.00   0.50    0.50    --  -42.49 -57.00   0.00  194
 19  ω   -113.00 -16.00   0.50    0.50    --  -42.49 -57.00  60.00  194
 20  ω   -113.00 -16.00   0.50    0.50    --  -42.49 -57.00-180.00  194
 21  ω    -30.00  65.00   0.50    0.50    --   42.49 -37.00  90.00  190
 22  ω     87.00 134.00   0.50    1.50    --  111.00  30.00 -30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0276939000
_diffrn_orient_matrix_UB_12      -0.0658534000
_diffrn_orient_matrix_UB_13      -0.1364334000
_diffrn_orient_matrix_UB_21      0.0168842000
_diffrn_orient_matrix_UB_22      0.0984178000
_diffrn_orient_matrix_UB_23      -0.1002524000
_diffrn_orient_matrix_UB_31      0.0539079000
_diffrn_orient_matrix_UB_32      -0.0646593000
_diffrn_orient_matrix_UB_33      -0.0134466000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2605
_reflns_number_total             2609

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.000188(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      1.215
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+13.9688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0519
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.82 with sigma of 0.001
 O7-H7B = O7-H7C = O7-H7A
 0.82 with sigma of 0.01
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.37621(15) 0.0019(3) 0.5766(4) 0.0255(8) Uani 1 1 d . . . . .
C2 C 0.31470(17) 0.1628(3) 0.4213(5) 0.0283(9) Uani 1 1 d . . . . .
C3 C 0.31004(15) 0.1336(3) 0.7055(4) 0.0250(7) Uani 1 1 d . . . . .
H4A H 0.4425(19) 0.155(2) 0.417(4) 0.037 Uiso 1 1 d D U . . .
H4B H 0.4609(10) 0.244(3) 0.506(4) 0.037 Uiso 1 1 d D U . . .
C4 C 0.33903(14) 0.4375(3) 0.5513(4) 0.0192(7) Uani 1 1 d . . . . .
H4 H 0.311491 0.410913 0.476560 0.023 Uiso 1 1 calc R U . . .
C5 C 0.34481(15) 0.5573(3) 0.5749(4) 0.0212(7) Uani 1 1 d . . . . .
C6 C 0.38517(16) 0.5947(3) 0.6846(4) 0.0237(7) Uani 1 1 d . . . . .
H6 H 0.390203 0.675906 0.704058 0.028 Uiso 1 1 calc R U . . .
C7 C 0.41810(15) 0.5134(3) 0.7655(4) 0.0218(7) Uani 1 1 d . . . . .
H7 H 0.445964 0.537747 0.840661 0.026 Uiso 1 1 calc R U . . .
C8 C 0.40940(13) 0.3959(3) 0.7342(4) 0.0164(6) Uani 1 1 d . . . . .
C9 C 0.44303(14) 0.3009(3) 0.8170(4) 0.0175(6) Uani 1 1 d . . . . .
C10 C 0.30855(17) 0.6420(4) 0.4820(5) 0.0297(8) Uani 1 1 d . . . . .
H10A H 0.281930 0.598315 0.414234 0.045 Uiso 1 1 calc R U . . .
H10B H 0.330852 0.691130 0.425207 0.045 Uiso 1 1 calc R U . . .
H10C H 0.289256 0.691569 0.545897 0.045 Uiso 1 1 calc R U . . .
N1 N 0.37047(11) 0.3575(2) 0.6288(3) 0.0158(5) Uani 1 1 d . . . . .
O1 O 0.38090(13) -0.0977(2) 0.5699(4) 0.0373(7) Uani 1 1 d . . . . .
O2 O 0.28317(15) 0.1614(3) 0.3187(4) 0.0462(9) Uani 1 1 d . . . . .
O3 O 0.27476(13) 0.1086(3) 0.7691(4) 0.0394(7) Uani 1 1 d . . . . .
O4 O 0.43348(10) 0.2126(2) 0.4627(3) 0.0218(5) Uani 1 1 d D . . . .
O5 O 0.47923(11) 0.3278(2) 0.9161(3) 0.0240(6) Uani 1 1 d . . . . .
O6 O 0.43057(10) 0.1962(2) 0.7744(3) 0.0186(5) Uani 1 1 d . . . . .
O7 O 0.47139(12) 0.0133(3) 0.3649(3) 0.0313(6) Uani 1 1 d D . . . .
H7A H 0.486(4) 0.026(9) 0.290(7) 0.047 Uiso 0.5 1 d D U P A -2
H7B H 0.489(4) 0.017(11) 0.448(6) 0.047 Uiso 0.5 1 d D U P B -1
H7C H 0.456(2) -0.050(3) 0.347(6) 0.047 Uiso 1 1 d D U . . .
Re1 Re 0.36778(2) 0.16873(2) 0.59284(2) 0.01680(8) 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
C1 O1 1.145(5) . ?
C1 Re1 1.924(4) . ?
C2 O2 1.141(5) . ?
C2 Re1 1.913(4) . ?
C3 O3 1.144(5) . ?
C3 Re1 1.904(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(5) . ?
C4 N1 1.341(4) . ?
C5 C6 1.387(5) . ?
C5 C10 1.505(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(5) . ?
C8 C9 1.510(5) . ?
C8 N1 1.345(4) . ?
C9 O5 1.228(4) . ?
C9 O6 1.283(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
N1 Re1 2.180(3) . ?
O4 H4A 0.8201(10) . ?
O4 H4B 0.8200(11) . ?
O4 Re1 2.188(3) . ?
O6 Re1 2.146(2) . ?
O7 H7A 0.825(10) . ?
O7 H7B 0.824(10) . ?
O7 H7C 0.825(10) . ?

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
O1 C1 Re1 178.5(4) . . ?
O2 C2 Re1 178.7(3) . . ?
O3 C3 Re1 177.1(3) . . ?
C5 C4 H4 118.4 . . ?
N1 C4 H4 118.4 . . ?
N1 C4 C5 123.1(3) . . ?
C4 C5 C10 120.2(3) . . ?
C6 C5 C4 117.7(3) . . ?
C6 C5 C10 122.1(3) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0(3) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.8 . . ?
C8 C7 C6 118.3(3) . . ?
C8 C7 H7 120.8 . . ?
C7 C8 C9 122.2(3) . . ?
N1 C8 C7 122.9(3) . . ?
N1 C8 C9 114.9(3) . . ?
O5 C9 C8 119.5(3) . . ?
O5 C9 O6 125.5(3) . . ?
O6 C9 C8 115.0(3) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 N1 C8 118.0(3) . . ?
C4 N1 Re1 126.1(2) . . ?
C8 N1 Re1 115.9(2) . . ?
H4A O4 H4B 109(4) . . ?
Re1 O4 H4A 111(3) . . ?
Re1 O4 H4B 117(3) . . ?
C9 O6 Re1 119.5(2) . . ?
H7A O7 H7C 103(8) . . ?
H7B O7 H7C 114(9) . . ?
C1 Re1 N1 171.48(13) . . ?
C1 Re1 O4 95.14(13) . . ?
C1 Re1 O6 97.46(13) . . ?
C2 Re1 C1 88.36(15) . . ?
C2 Re1 N1 99.40(13) . . ?
C2 Re1 O4 92.29(15) . . ?
C2 Re1 O6 172.70(13) . . ?
C3 Re1 C1 85.93(16) . . ?
C3 Re1 C2 87.38(17) . . ?
C3 Re1 N1 97.88(13) . . ?
C3 Re1 O4 178.88(13) . . ?
C3 Re1 O6 97.40(13) . . ?
N1 Re1 O4 81.11(10) . . ?
O6 Re1 N1 74.55(10) . . ?
O6 Re1 O4 82.82(9) . . ?

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
C4 C5 C6 C7 0.2(5) . . . . ?
C5 C4 N1 C8 -0.1(5) . . . . ?
C5 C4 N1 Re1 -176.5(3) . . . . ?
C5 C6 C7 C8 -0.2(5) . . . . ?
C6 C7 C8 C9 -179.7(3) . . . . ?
C6 C7 C8 N1 0.0(5) . . . . ?
C7 C8 C9 O5 0.4(5) . . . . ?
C7 C8 C9 O6 -179.3(3) . . . . ?
C7 C8 N1 C4 0.1(5) . . . . ?
C7 C8 N1 Re1 176.9(3) . . . . ?
C8 C9 O6 Re1 2.0(4) . . . . ?
C9 C8 N1 C4 179.9(3) . . . . ?
C9 C8 N1 Re1 -3.4(4) . . . . ?
C10 C5 C6 C7 -178.9(4) . . . . ?
N1 C4 C5 C6 -0.1(5) . . . . ?
N1 C4 C5 C10 179.1(3) . . . . ?
N1 C8 C9 O5 -179.4(3) . . . . ?
N1 C8 C9 O6 1.0(4) . . . . ?
O5 C9 O6 Re1 -177.6(3) . . . . ?


####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 2205510'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 N2 O8 Re'
_chemical_formula_sum            'C9 H5 N2 O8 Re'
_chemical_formula_weight         455.35
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.79860(10)
_cell_length_b                   18.1770(3)
_cell_length_c                   9.65140(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.9710(10)
_cell_angle_gamma                90
_cell_volume                     1188.22(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9348
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.2300
_cell_measurement_theta_min      2.4020
_shelx_estimated_absorpt_T_max   0.193
_shelx_estimated_absorpt_T_min   0.076
_exptl_absorpt_coefficient_mu    20.464
_exptl_absorpt_correction_T_max  0.258
_exptl_absorpt_correction_T_min  0.028
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             848
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -3 -5 0.0596
4 1 -3 0.1064
-2 0 1 0.1226
0 5 -2 0.0539
0 -5 2 0.0668
0 1 1 0.0552
0 -5 -1 0.0721
-4 -4 1 0.1046
3 5 -1 0.1129
-2 -5 -5 0.0704
1 -4 -5 0.0664
2 -1 1 0.1291
0 5 1 0.0574

_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12

_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11577
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.486
_diffrn_reflns_theta_min         4.866
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     27.00  97.40   0.80    0.80    --   42.49-125.00 -60.00   88
  2  ω    -44.00 128.00   0.80    0.80    --   42.49   0.00 -30.00  215
  3  ω      6.00  82.00   0.80    0.80    --   42.49 -99.00 -30.00   95
  4  ω     87.00 177.40   0.80    0.80    --  111.00  30.00 150.00  113
  5  ω    104.00 177.60   0.80    0.80    --  111.00 111.00  90.00   92
  6  ω     61.00 145.00   0.80    0.80    --  111.00 178.00 -30.00  105
  7  ω    103.00 177.40   0.80    0.80    --  111.00  77.00-180.00   93
  8  ω     36.00 108.00   0.80    0.80    --  111.00-111.00 -60.00   90
  9  ω    103.00 177.40   0.80    0.80    --  111.00  77.00 -90.00   93
 10  ω     40.00 134.40   0.80    0.80    --  111.00 -45.00 -30.00  118
 11  ω     83.00 177.40   0.80    0.80    --  111.00  61.00-150.00  118
 12  ω     36.00 108.00   0.80    0.80    --  111.00-111.00  30.00   90
 13  ω   -113.00 -17.00   0.80    0.80    --  -42.49 -57.00 150.00  120
 14  ω   -115.00 -20.60   0.80    0.80    --  -42.49 -37.00  30.00  118
 15  ω     16.00 112.00   0.80    0.80    --   42.49  57.00   0.00  120
 16  ω     87.00 177.40   0.80    0.80    --  111.00  45.00 -90.00  113
 17  ω    103.00 177.40   0.80    0.80    --  111.00  77.00 -60.00   93
 18  ω     30.00 106.00   0.80    0.80    --  111.00 -94.00 120.00   95
 19  ω     66.00 178.00   0.80    0.80    --  111.00  15.00  60.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0992198000
_diffrn_orient_matrix_UB_12      0.0528818000
_diffrn_orient_matrix_UB_13      0.1094921000
_diffrn_orient_matrix_UB_21      -0.2026180000
_diffrn_orient_matrix_UB_22      0.0167686000
_diffrn_orient_matrix_UB_23      0.0530486000
_diffrn_orient_matrix_UB_31      0.0290571000
_diffrn_orient_matrix_UB_32      -0.0640389000
_diffrn_orient_matrix_UB_33      0.1043052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2411
_reflns_number_total             2423

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.889
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00180(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2423
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.225
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0292P)²+1.7966P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0556
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O4-H4A
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.8768(6) 0.5431(2) 0.7898(4) 0.0259(7) Uani 1 1 d . . . . .
C2 C 1.0324(5) 0.41090(19) 0.8423(4) 0.0227(7) Uani 1 1 d . . . . .
C3 C 0.7041(6) 0.44758(18) 0.9560(4) 0.0241(8) Uani 1 1 d . . . . .
C4 C 0.7174(5) 0.2723(2) 0.7638(4) 0.0245(7) Uani 1 1 d . . . . .
H4 H 0.836855 0.270790 0.822539 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6289(5) 0.2064(2) 0.7193(4) 0.0281(7) Uani 1 1 d . . . . .
H5 H 0.686876 0.160731 0.747873 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4553(5) 0.2081(2) 0.6330(4) 0.0268(7) Uani 1 1 d . . . . .
H6 H 0.393244 0.164207 0.598283 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3763(5) 0.27681(19) 0.5994(3) 0.0211(6) Uani 1 1 d . . . . .
C8 C 0.4675(5) 0.34130(18) 0.6455(3) 0.0198(6) Uani 1 1 d . . . . .
C9 C 0.3909(5) 0.41807(19) 0.6141(3) 0.0191(6) Uani 1 1 d . . . . .
N1 N 0.6398(4) 0.33720(15) 0.7265(3) 0.0207(5) Uani 1 1 d . . . . .
N2 N 0.1898(5) 0.27793(16) 0.5097(3) 0.0251(6) Uani 1 1 d . . . . .
O1 O 0.9349(4) 0.60198(14) 0.8020(3) 0.0353(6) Uani 1 1 d . . . . .
O2 O 1.1858(4) 0.38981(15) 0.8850(3) 0.0293(5) Uani 1 1 d . . . . .
O3 O 0.6601(5) 0.44866(14) 1.0687(3) 0.0295(6) Uani 1 1 d . . . . .
O4 O 0.8286(4) 0.43328(16) 0.5488(3) 0.0236(5) Uani 1 1 d D . . . .
H4A H 0.938(4) 0.424(3) 0.525(6) 0.049(16) Uiso 1 1 d D . . . .
H4B H 0.807(9) 0.474(3) 0.520(6) 0.051(17) Uiso 1 1 d . . . . .
O5 O 0.2336(4) 0.42618(14) 0.5404(3) 0.0238(5) Uani 1 1 d . . . . .
O6 O 0.4967(3) 0.46988(13) 0.6673(2) 0.0220(5) Uani 1 1 d . . . . .
O7 O 0.2000(4) 0.27405(17) 0.3855(3) 0.0373(6) Uani 1 1 d . . . . .
O8 O 0.0362(4) 0.28018(19) 0.5665(3) 0.0404(7) Uani 1 1 d . . . . .
Re1 Re 0.77794(2) 0.44390(2) 0.77050(2) 0.01855(9) 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
C1 O1 1.143(5) . ?
C1 Re1 1.928(4) . ?
C2 O2 1.154(4) . ?
C2 Re1 1.904(4) . ?
C3 O3 1.153(5) . ?
C3 Re1 1.902(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(5) . ?
C4 N1 1.330(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(5) . ?
C7 C8 1.382(5) . ?
C7 N2 1.472(4) . ?
C8 C9 1.511(4) . ?
C8 N1 1.352(4) . ?
C9 O5 1.241(4) . ?
C9 O6 1.266(4) . ?
N1 Re1 2.181(3) . ?
N2 O7 1.209(4) . ?
N2 O8 1.221(4) . ?
O4 H4A 0.818(10) . ?
O4 H4B 0.80(6) . ?
O4 Re1 2.205(3) . ?
O6 Re1 2.131(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
O1 C1 Re1 179.6(4) . . ?
O2 C2 Re1 178.9(3) . . ?
O3 C3 Re1 178.9(3) . . ?
C5 C4 H4 119.0 . . ?
N1 C4 H4 119.0 . . ?
N1 C4 C5 122.0(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 H5 120.3 . . ?
C5 C6 H6 121.5 . . ?
C5 C6 C7 117.0(3) . . ?
C7 C6 H6 121.5 . . ?
C6 C7 N2 116.5(3) . . ?
C8 C7 C6 122.3(3) . . ?
C8 C7 N2 121.2(3) . . ?
C7 C8 C9 125.6(3) . . ?
N1 C8 C7 118.8(3) . . ?
N1 C8 C9 115.7(3) . . ?
O5 C9 C8 119.3(3) . . ?
O5 C9 O6 125.1(3) . . ?
O6 C9 C8 115.6(3) . . ?
C4 N1 C8 120.6(3) . . ?
C4 N1 Re1 125.6(2) . . ?
C8 N1 Re1 113.6(2) . . ?
O7 N2 C7 117.5(3) . . ?
O7 N2 O8 124.9(3) . . ?
O8 N2 C7 117.6(3) . . ?
H4A O4 H4B 104(5) . . ?
Re1 O4 H4A 121(4) . . ?
Re1 O4 H4B 103(4) . . ?
C9 O6 Re1 118.7(2) . . ?
C1 Re1 N1 172.51(13) . . ?
C1 Re1 O4 95.36(13) . . ?
C1 Re1 O6 97.42(13) . . ?
C2 Re1 C1 87.78(15) . . ?
C2 Re1 N1 98.81(12) . . ?
C2 Re1 O4 96.42(13) . . ?
C2 Re1 O6 171.92(12) . . ?
C3 Re1 C1 89.66(15) . . ?
C3 Re1 C2 88.52(16) . . ?
C3 Re1 N1 94.05(13) . . ?
C3 Re1 O4 173.07(14) . . ?
C3 Re1 O6 97.65(13) . . ?
N1 Re1 O4 80.44(10) . . ?
O6 Re1 N1 75.65(10) . . ?
O6 Re1 O4 77.00(10) . . ?

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
O4 H4A O5 0.818(10) 2.00(3) 2.765(4) 155(6) 1_655 yes
O4 H4B O5 0.80(6) 1.92(6) 2.717(4) 176(6) 3_666 yes

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
C4 C5 C6 C7 -2.0(6) . . . . ?
C5 C4 N1 C8 1.5(5) . . . . ?
C5 C4 N1 Re1 -173.2(3) . . . . ?
C5 C6 C7 C8 1.9(5) . . . . ?
C5 C6 C7 N2 -178.9(3) . . . . ?
C6 C7 C8 C9 -179.8(3) . . . . ?
C6 C7 C8 N1 -0.1(5) . . . . ?
C6 C7 N2 O7 -84.1(4) . . . . ?
C6 C7 N2 O8 93.5(4) . . . . ?
C7 C8 C9 O5 -0.3(5) . . . . ?
C7 C8 C9 O6 179.6(3) . . . . ?
C7 C8 N1 C4 -1.7(5) . . . . ?
C7 C8 N1 Re1 173.7(2) . . . . ?
C8 C7 N2 O7 95.1(4) . . . . ?
C8 C7 N2 O8 -87.3(4) . . . . ?
C8 C9 O6 Re1 7.2(4) . . . . ?
C9 C8 N1 C4 178.0(3) . . . . ?
C9 C8 N1 Re1 -6.6(3) . . . . ?
N1 C4 C5 C6 0.4(6) . . . . ?
N1 C8 C9 O5 180.0(3) . . . . ?
N1 C8 C9 O6 -0.1(4) . . . . ?
N2 C7 C8 C9 1.1(5) . . . . ?
N2 C7 C8 N1 -179.3(3) . . . . ?
O5 C9 O6 Re1 -172.9(3) . . . . ?


####################################################################### 
# 
# 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_23
_database_code_depnum_ccdc_archive 'CCDC 2205513'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 Cl N O6 Re'
_chemical_formula_sum            'C9 H5 Cl N O6 Re'
_chemical_formula_weight         444.79
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.3055(2)
_cell_length_b                   9.8069(2)
_cell_length_c                   10.5545(2)
_cell_angle_alpha                102.051(2)
_cell_angle_beta                 100.494(2)
_cell_angle_gamma                105.893(2)
_cell_volume                     593.68(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8064
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1100
_cell_measurement_theta_min      4.4190
_shelx_estimated_absorpt_T_max   0.554
_shelx_estimated_absorpt_T_min   0.060
_exptl_absorpt_coefficient_mu    22.318
_exptl_absorpt_correction_T_max  0.539
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0204
0 0 -1 0.0104
0 -5 2 0.0489
0 5 -2 0.0489
4 -3 -1 0.1297
-4 3 1 0.1297

_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03

_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11168
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.481
_diffrn_reflns_theta_min         4.429
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -129.00  44.00   1.00    1.00    --  -42.49   0.00-150.00  173
  2  ω     27.00  98.00   1.00    1.00    --   42.49-125.00-150.00   71
  3  ω     25.00  96.00   1.00    1.00    --   42.49-122.00 157.00   71
  4  ω     20.00 115.00   1.00    1.00    --   42.49  37.00  60.00   95
  5  ω     27.00  98.00   1.00    1.00    --   42.49-125.00 -30.00   71
  6  ω    103.00 178.00   1.00    1.50    --  111.00  77.00 120.00   75
  7  ω     40.00 135.00   1.00    1.50    --  111.00 -45.00  60.00   95
  8  ω     31.00 156.00   1.00    1.50    --  111.00 -15.00 150.00  125
  9  ω     41.00 139.00   1.00    1.50    --  111.00 -61.00   0.00   98
 10  ω     39.00 111.00   1.00    1.50    --  111.00-122.00 157.00   72
 11  ω     36.00 109.00   1.00    1.50    --  111.00-111.00  90.00   73
 12  ω     30.00 107.00   1.00    1.50    --  111.00 -94.00 -90.00   77
 13  ω     36.00 109.00   1.00    1.50    --  111.00-111.00-120.00   73
 14  ω    103.00 178.00   1.00    1.50    --  111.00  77.00  60.00   75
 15  ω     30.00 107.00   1.00    1.50    --  111.00 -94.00 -30.00   77
 16  ω    104.00 178.00   1.00    1.50    --  111.00 111.00 150.00   74
 17  ω     83.00 178.00   1.00    1.50    --  111.00  61.00-150.00   95
 18  ω     37.00 142.00   1.00    1.50    --  111.00 -77.00 120.00  105
 19  ω    103.00 178.00   1.00    1.50    --  111.00  77.00 150.00   75
 20  ω     37.00 142.00   1.00    1.50    --  111.00 -77.00 -30.00  105
 21  ω   -113.00 -16.00   1.00    1.00    --  -42.49 -57.00-180.00   97
 22  ω    -69.00  28.00   1.00    1.00    --  -42.49  57.00 -30.00   97
 23  ω     10.00  42.00   1.00    1.00    --   42.49  81.00-147.15   32
 24  ω     11.00  42.00   1.00    1.00    --   42.49  77.00 -43.62   31
 25  ω     16.00 113.00   1.00    1.00    --   42.49  57.00 150.00   97
 26  ω     10.00  42.00   1.00    1.00    --   42.49  82.00  77.39   32
 27  ω     66.00 178.00   1.00    1.50    --  111.00  15.00 -30.00  112
 28  ω     83.00 178.00   1.00    1.50    --  111.00  64.00 167.82   95
 29  ω     83.00 178.00   1.00    1.50    --  111.00  61.00-125.02   95
 30  ω     83.00 178.00   1.00    1.50    --  111.00  61.00  60.00   95
 31  ω     82.00 178.00   1.00    1.50    --  111.00  67.00 120.03   96
 32  ω     83.00 178.00   1.00    1.50    --  111.00  61.00 -30.00   95
 33  ω     83.00 178.00   1.00    1.50    --  111.00  61.00  90.00   95
 34  ω     84.00 178.00   1.00    1.50    --  111.00  60.00  -8.59   94
 35  ω     83.00 178.00   1.00    1.50    --  111.00  61.00 -60.00   95
 36  ω     84.00 178.00   1.00    1.50    --  111.00  59.00 -78.48   94
 37  ω     87.00 178.00   1.00    1.50    --  111.00  45.00  30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203454000
_diffrn_orient_matrix_UB_12      -0.0799581000
_diffrn_orient_matrix_UB_13      -0.1459712000
_diffrn_orient_matrix_UB_21      -0.2079290000
_diffrn_orient_matrix_UB_22      0.0471346000
_diffrn_orient_matrix_UB_23      -0.0475202000
_diffrn_orient_matrix_UB_31      0.1592189000
_diffrn_orient_matrix_UB_32      0.1421935000
_diffrn_orient_matrix_UB_33      -0.0159238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2395
_reflns_number_total             2415

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00057(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2415
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0185
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+0.5594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0482
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-H4A \\sim O4-H4B
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
C2 \\sim O2: within 3A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 3A
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.7633(6) 0.7098(4) 0.1917(3) 0.0240(7) Uani 1 1 d . . . . .
C2 C 1.0178(6) 0.5743(5) 0.3149(3) 0.0307(8) Uani 1 1 d . U . . .
H4A H 0.724(8) 0.438(5) -0.019(4) 0.037 Uiso 1 1 d D U . . .
H4B H 0.803(8) 0.356(5) 0.049(5) 0.037 Uiso 1 1 d D U . . .
C3 C 0.6841(5) 0.6182(4) 0.4053(3) 0.0210(6) Uani 1 1 d . . . . .
C4 C 0.6985(6) 0.2354(4) 0.3238(3) 0.0205(6) Uani 1 1 d . . . . .
H4 H 0.854940 0.286113 0.367238 0.025 Uiso 1 1 calc R U . . .
C5 C 0.5976(6) 0.0938(4) 0.3322(3) 0.0243(6) Uani 1 1 d . . . . .
C6 C 0.3760(7) 0.0151(4) 0.2641(3) 0.0294(7) Uani 1 1 d . . . . .
H6 H 0.309449 -0.083844 0.265469 0.035 Uiso 1 1 calc R U . . .
C7 C 0.2517(6) 0.0843(4) 0.1931(3) 0.0241(6) Uani 1 1 d . . . . .
H7 H 0.097151 0.033538 0.145262 0.029 Uiso 1 1 calc R U . . .
C8 C 0.3551(5) 0.2275(3) 0.1927(3) 0.0161(5) Uani 1 1 d . . . . .
C9 C 0.2249(5) 0.3141(3) 0.1285(3) 0.0155(5) Uani 1 1 d . . . . .
Cl1 Cl 0.75962(17) 0.02246(10) 0.43347(9) 0.0356(2) Uani 1 1 d . . . . .
N1 N 0.5763(4) 0.3012(3) 0.2546(2) 0.0158(5) Uani 1 1 d . . . . .
O1 O 0.7954(6) 0.8206(3) 0.1670(3) 0.0385(7) Uani 1 1 d . . . . .
O2 O 1.2075(5) 0.6094(4) 0.3679(3) 0.0528(9) Uani 1 1 d . U . . .
O3 O 0.6873(4) 0.6760(3) 0.5133(2) 0.0300(5) Uani 1 1 d . . . . .
O4 O 0.7123(4) 0.3958(2) 0.0389(2) 0.0187(4) Uani 1 1 d D . . . .
O5 O 0.0190(4) 0.2590(2) 0.0798(2) 0.0222(4) Uani 1 1 d . . . . .
O6 O 0.3452(4) 0.4448(2) 0.1330(2) 0.0157(4) Uani 1 1 d . . . . .
Re1 Re 0.70161(2) 0.52283(2) 0.23313(2) 0.01485(8) 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
C1 O1 1.144(5) . ?
C1 Re1 1.926(4) . ?
C2 O2 1.146(5) . ?
C2 Re1 1.901(4) . ?
C3 O3 1.156(4) . ?
C3 Re1 1.900(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(5) . ?
C4 N1 1.345(4) . ?
C5 C6 1.369(5) . ?
C5 Cl1 1.727(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(4) . ?
C8 C9 1.508(4) . ?
C8 N1 1.347(4) . ?
C9 O5 1.224(4) . ?
C9 O6 1.284(4) . ?
N1 Re1 2.174(3) . ?
O4 H4A 0.81(4) . ?
O4 H4B 0.78(4) . ?
O4 Re1 2.189(2) . ?
O6 Re1 2.147(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
O1 C1 Re1 178.6(3) . . ?
O2 C2 Re1 177.5(3) . . ?
O3 C3 Re1 175.6(3) . . ?
C5 C4 H4 119.7 . . ?
N1 C4 H4 119.7 . . ?
N1 C4 C5 120.5(3) . . ?
C4 C5 Cl1 117.6(3) . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 Cl1 121.5(3) . . ?
C5 C6 H6 121.0 . . ?
C5 C6 C7 118.0(3) . . ?
C7 C6 H6 121.0 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 122.1(3) . . ?
N1 C8 C7 122.2(3) . . ?
N1 C8 C9 115.7(3) . . ?
O5 C9 C8 119.6(3) . . ?
O5 C9 O6 125.4(3) . . ?
O6 C9 C8 115.0(3) . . ?
C4 N1 C8 119.1(3) . . ?
C4 N1 Re1 125.9(2) . . ?
C8 N1 Re1 115.06(19) . . ?
H4A O4 H4B 112(5) . . ?
Re1 O4 H4A 118(3) . . ?
Re1 O4 H4B 110(4) . . ?
C9 O6 Re1 118.91(18) . . ?
C1 Re1 N1 170.15(12) . . ?
C1 Re1 O4 96.01(11) . . ?
C1 Re1 O6 95.21(12) . . ?
C2 Re1 C1 88.70(17) . . ?
C2 Re1 N1 100.75(15) . . ?
C2 Re1 O4 95.78(12) . . ?
C2 Re1 O6 174.76(12) . . ?
C3 Re1 C1 88.65(14) . . ?
C3 Re1 C2 84.87(14) . . ?
C3 Re1 N1 94.88(12) . . ?
C3 Re1 O4 175.30(11) . . ?
C3 Re1 O6 98.67(11) . . ?
N1 Re1 O4 80.43(9) . . ?
O6 Re1 N1 75.18(9) . . ?
O6 Re1 O4 80.37(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
O4 H4A O6 0.81(4) 1.90(4) 2.669(3) 157(5) 2_665 yes
O4 H4B O5 0.78(4) 1.88(4) 2.662(3) 178(5) 1_655 yes

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
C4 C5 C6 C7 -3.7(5) . . . . ?
C5 C4 N1 C8 -0.4(4) . . . . ?
C5 C4 N1 Re1 178.8(2) . . . . ?
C5 C6 C7 C8 0.5(5) . . . . ?
C6 C7 C8 C9 -174.3(3) . . . . ?
C6 C7 C8 N1 2.8(5) . . . . ?
C7 C8 C9 O5 3.2(4) . . . . ?
C7 C8 C9 O6 -178.3(3) . . . . ?
C7 C8 N1 C4 -2.9(4) . . . . ?
C7 C8 N1 Re1 177.8(2) . . . . ?
C8 C9 O6 Re1 -1.8(3) . . . . ?
C9 C8 N1 C4 174.4(2) . . . . ?
C9 C8 N1 Re1 -4.9(3) . . . . ?
Cl1 C5 C6 C7 175.1(3) . . . . ?
N1 C4 C5 C6 3.8(5) . . . . ?
N1 C4 C5 Cl1 -175.1(2) . . . . ?
N1 C8 C9 O5 -174.1(2) . . . . ?
N1 C8 C9 O6 4.4(4) . . . . ?
O5 C9 O6 Re1 176.7(2) . . . . ?

####################################################################### 
# 
# 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_24
_database_code_depnum_ccdc_archive 'CCDC 2205514'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H5 F3 N O6 Re'
_chemical_formula_sum            'C10 H5 F3 N O6 Re'
_chemical_formula_weight         478.35
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.42250(10)
_cell_length_b                   10.7862(3)
_cell_length_c                   18.6703(5)
_cell_angle_alpha                83.339(2)
_cell_angle_beta                 85.503(2)
_cell_angle_gamma                79.429(2)
_cell_volume                     1260.68(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21715
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.7820
_cell_measurement_theta_min      4.1770
_shelx_estimated_absorpt_T_max   0.696
_shelx_estimated_absorpt_T_min   0.119
_exptl_absorpt_coefficient_mu    19.543
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0093
0 0 1 0.0063
0 -1 0 0.0116
0 1 0 0.0116
4 1 1 0.1004
-4 -1 -1 0.0854

_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02

_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25823
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.500
_diffrn_reflns_theta_min         2.387
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00 125.00   0.50    0.20    --   51.79  77.00  30.00  192
  2  ω     29.00 125.00   0.50    0.20    --   51.79  77.00 120.00  192
  3  ω     85.00 178.00   0.50    0.40    --  107.75  77.00 -60.00  186
  4  ω     30.00 125.00   0.50    0.20    --   51.79  76.00-172.00  190
  5  ω     86.00 178.00   0.50    0.40    --  107.75  76.00-172.00  184
  6  ω     94.00 178.00   0.50    0.40    --  107.75  30.00 -90.00  168
  7  ω     96.00 178.00   0.50    0.40    --  107.75  15.00  90.00  164
  8  ω     96.00 178.00   0.50    0.40    --  107.75  15.00 120.00  164
  9  ω    102.00 178.00   0.50    0.40    --  107.75 111.00   0.00  152
 10  ω     62.00 146.00   0.50    0.40    --  107.75 178.00   0.00  168
 11  ω    102.00 178.00   0.50    0.40    --  107.75 111.00 -30.00  152
 12  ω    102.00 178.00   0.50    0.40    --  107.75 111.00 -60.00  152
 13  ω     37.00 124.00   0.50    0.40    --  107.75 -61.00  60.00  174
 14  ω     35.00 130.00   0.50    0.40    --  107.75 -76.00  61.00  190
 15  ω     34.00 130.00   0.50    0.40    --  107.75 -77.00   0.00  192
 16  ω    -21.00  74.00   0.50    0.20    --   51.79 -76.00  61.00  190
 17  ω     31.00 106.00   0.50    0.40    --  107.75 -94.00 -60.00  150
 18  ω     31.00 106.00   0.50    0.40    --  107.75 -94.00-120.00  150
 19  ω     31.00 109.00   0.50    0.40    --  107.75-111.00-180.00  156
 20  ω     31.00 106.00   0.50    0.40    --  107.75 -94.00  60.00  150
 21  ω     31.00 106.00   0.50    0.40    --  107.75 -94.00   0.00  150
 22  ω     31.00 109.00   0.50    0.40    --  107.75-111.00 -30.00  156
 23  ω     31.00 106.00   0.50    0.40    --  107.75 -94.00 -90.00  150
 24  ω   -124.00 -37.00   0.50    0.20    --  -51.79 -57.00 -60.00  174
 25  ω   -124.00 -37.00   0.50    0.20    --  -51.79 -57.00 -90.00  174
 26  ω   -124.00 -37.00   0.50    0.20    --  -51.79 -57.00-150.00  174
 27  ω   -159.00 -64.00   0.50    0.40    --  -86.25 -76.00  61.00  190
 28  ω   -125.00 -30.00   0.50    0.20    --  -51.79 -76.00  61.00  190
 29  ω   -125.00 -29.00   0.50    0.20    --  -51.79 -77.00   0.00  192
 30  ω    -64.00  26.00   0.50    0.20    --  -51.79  37.00-150.00  180
 31  ω    -74.00  21.00   0.50    0.20    --  -51.79  76.00-172.00  190
 32  ω   -108.00 -13.00   0.50    0.40    --  -86.25  76.00-172.00  190
 33  ω    -99.00 -10.00   0.50    0.40    --  -86.25  45.00  30.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1253161000
_diffrn_orient_matrix_UB_12      0.1210234000
_diffrn_orient_matrix_UB_13      -0.0392267000
_diffrn_orient_matrix_UB_21      0.0559163000
_diffrn_orient_matrix_UB_22      0.0787612000
_diffrn_orient_matrix_UB_23      0.0571910000
_diffrn_orient_matrix_UB_31      0.2022764000
_diffrn_orient_matrix_UB_32      0.0221216000
_diffrn_orient_matrix_UB_33      -0.0459952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4813
_reflns_number_total             5099

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.000196(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0146
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0125P)²+1.3370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0336
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B = O10-H10A = O10-H10B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C14(H14), C16(H16), C17(H17)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.24671(2) 0.81725(2) 0.61950(2) 0.01221(4) Uani 1 1 d . . . . .
F1 F 0.2574(3) 0.73753(18) 0.26809(8) 0.0319(4) Uani 1 1 d . . . . .
F2 F 0.0203(3) 0.65361(19) 0.33243(9) 0.0391(4) Uani 1 1 d . . . . .
F3 F 0.0208(3) 0.85187(18) 0.33115(10) 0.0449(5) Uani 1 1 d . . . . .
O1 O 0.1730(3) 0.8998(2) 0.77283(11) 0.0363(5) Uani 1 1 d . . . . .
O2 O -0.2045(3) 0.9481(2) 0.58910(13) 0.0339(5) Uani 1 1 d . . . . .
O3 O 0.3572(3) 1.07709(18) 0.56780(12) 0.0301(4) Uani 1 1 d . . . . .
O4 O 0.1648(3) 0.62837(17) 0.65001(9) 0.0161(3) Uani 1 1 d D . . . .
O5 O 0.8494(3) 0.61052(17) 0.57014(9) 0.0201(4) Uani 1 1 d . . . . .
O6 O 0.5644(3) 0.71091(16) 0.62972(9) 0.0151(3) Uani 1 1 d . . . . .
N1 N 0.3340(3) 0.74162(18) 0.51559(10) 0.0131(4) Uani 1 1 d . . . . .
C1 C 0.2005(4) 0.8686(3) 0.71609(14) 0.0211(5) Uani 1 1 d . . . . .
C2 C -0.0353(4) 0.8976(2) 0.60212(13) 0.0199(5) Uani 1 1 d . . . . .
C3 C 0.3242(4) 0.9777(3) 0.58708(14) 0.0199(5) Uani 1 1 d . . . . .
C4 C 0.2124(4) 0.7595(2) 0.45903(13) 0.0155(5) Uani 1 1 d . . . . .
H4 H 0.071041 0.804434 0.463670 0.019 Uiso 1 1 calc R U . . .
C5 C 0.2885(4) 0.7135(2) 0.39344(13) 0.0167(5) Uani 1 1 d . . . . .
C6 C 0.4932(4) 0.6449(2) 0.38648(13) 0.0185(5) Uani 1 1 d . . . . .
H6 H 0.547142 0.612381 0.342252 0.022 Uiso 1 1 calc R U . . .
C7 C 0.6167(4) 0.6251(2) 0.44594(13) 0.0165(5) Uani 1 1 d . . . . .
H7 H 0.756501 0.577402 0.443427 0.020 Uiso 1 1 calc R U . . .
C8 C 0.5335(4) 0.6758(2) 0.50861(12) 0.0134(4) Uani 1 1 d . . . . .
C9 C 0.6635(4) 0.6635(2) 0.57377(13) 0.0147(5) Uani 1 1 d . . . . .
C10 C 0.1478(4) 0.7400(3) 0.33100(13) 0.0214(5) Uani 1 1 d . . . . .
Re2 Re 0.24721(2) 0.39300(2) 0.14904(2) 0.01362(4) Uani 1 1 d . . . . .
F4 F 0.3279(4) 0.8752(2) -0.02318(11) 0.0594(6) Uani 1 1 d . . . . .
F5 F 0.2000(3) 1.02076(16) 0.04309(11) 0.0416(4) Uani 1 1 d . . . . .
F6 F 0.4826(3) 0.8945(2) 0.07129(14) 0.0632(7) Uani 1 1 d . . . . .
O7 O 0.3470(4) 0.1058(2) 0.19163(14) 0.0431(6) Uani 1 1 d . . . . .
O8 O 0.6833(3) 0.3908(2) 0.07158(11) 0.0365(5) Uani 1 1 d . . . . .
O9 O 0.1273(3) 0.3356(2) 0.00317(11) 0.0334(5) Uani 1 1 d . . . . .
O10 O 0.3310(3) 0.44621(17) 0.25104(9) 0.0169(3) Uani 1 1 d D . . . .
O11 O -0.3535(3) 0.57316(17) 0.22128(9) 0.0197(4) Uani 1 1 d . . . . .
O12 O -0.0635(2) 0.42730(16) 0.20479(9) 0.0152(3) Uani 1 1 d . . . . .
N2 N 0.1430(3) 0.59802(19) 0.13089(10) 0.0145(4) Uani 1 1 d . . . . .
C11 C 0.3110(4) 0.2131(3) 0.17591(15) 0.0250(6) Uani 1 1 d . . . . .
C12 C 0.5218(4) 0.3871(3) 0.10253(13) 0.0216(5) Uani 1 1 d . . . . .
C13 C 0.1647(4) 0.3579(3) 0.05876(14) 0.0218(5) Uani 1 1 d . . . . .
C14 C 0.2501(4) 0.6829(2) 0.09501(12) 0.0176(5) Uani 1 1 d . . . . .
H14 H 0.386655 0.654276 0.073289 0.021 Uiso 1 1 calc R U . . .
C15 C 0.1683(4) 0.8118(2) 0.08841(13) 0.0192(5) Uani 1 1 d . . . . .
C16 C -0.0290(4) 0.8561(3) 0.12070(14) 0.0205(5) Uani 1 1 d . . . . .
H16 H -0.085469 0.944206 0.117834 0.025 Uiso 1 1 calc R U . . .
C17 C -0.1408(4) 0.7678(2) 0.15721(13) 0.0184(5) Uani 1 1 d . . . . .
H17 H -0.277025 0.794365 0.179734 0.022 Uiso 1 1 calc R U . . .
C18 C -0.0528(4) 0.6412(2) 0.16059(12) 0.0144(5) Uani 1 1 d . . . . .
C19 C -0.1684(4) 0.5407(2) 0.19811(12) 0.0155(5) Uani 1 1 d . . . . .
C20 C 0.2957(4) 0.9006(3) 0.04549(16) 0.0276(6) Uani 1 1 d . . . . .
H4A H 0.063(4) 0.621(4) 0.6283(18) 0.041 Uiso 1 1 d D U . . .
H4B H 0.140(6) 0.619(4) 0.6936(6) 0.041 Uiso 1 1 d D U . . .
H10A H 0.350(6) 0.393(3) 0.2858(13) 0.041 Uiso 1 1 d D U . . .
H10B H 0.431(4) 0.484(3) 0.243(2) 0.041 Uiso 1 1 d D 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 O4 2.1974(17) . ?
Re1 O6 2.1602(16) . ?
Re1 N1 2.1845(19) . ?
Re1 C1 1.932(3) . ?
Re1 C2 1.894(3) . ?
Re1 C3 1.906(3) . ?
F1 C10 1.321(3) . ?
F2 C10 1.346(3) . ?
F3 C10 1.327(3) . ?
O1 C1 1.140(3) . ?
O2 C2 1.153(3) . ?
O3 C3 1.143(3) . ?
O4 H4A 0.816(10) . ?
O4 H4B 0.816(10) . ?
O5 C9 1.226(3) . ?
O6 C9 1.288(3) . ?
N1 C4 1.338(3) . ?
N1 C8 1.350(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(3) . ?
C5 C6 1.390(3) . ?
C5 C10 1.500(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(3) . ?
C8 C9 1.509(3) . ?
Re2 O10 2.1848(17) . ?
Re2 O12 2.1667(16) . ?
Re2 N2 2.184(2) . ?
Re2 C11 1.924(3) . ?
Re2 C12 1.897(3) . ?
Re2 C13 1.904(3) . ?
F4 C20 1.334(4) . ?
F5 C20 1.326(3) . ?
F6 C20 1.316(3) . ?
O7 C11 1.145(4) . ?
O8 C12 1.152(3) . ?
O9 C13 1.145(3) . ?
O10 H10A 0.817(10) . ?
O10 H10B 0.820(10) . ?
O11 C19 1.235(3) . ?
O12 C19 1.281(3) . ?
N2 C14 1.333(3) . ?
N2 C18 1.357(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.388(4) . ?
C15 C16 1.386(4) . ?
C15 C20 1.495(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.375(3) . ?
C18 C19 1.501(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Re1 O4 81.73(6) . . ?
O6 Re1 N1 74.96(7) . . ?
N1 Re1 O4 82.33(7) . . ?
C1 Re1 O4 94.91(9) . . ?
C1 Re1 O6 97.85(9) . . ?
C1 Re1 N1 172.58(9) . . ?
C2 Re1 O4 94.66(9) . . ?
C2 Re1 O6 173.15(9) . . ?
C2 Re1 N1 98.85(9) . . ?
C2 Re1 C1 88.23(11) . . ?
C2 Re1 C3 86.10(11) . . ?
C3 Re1 O4 176.31(9) . . ?
C3 Re1 O6 97.14(8) . . ?
C3 Re1 N1 93.98(9) . . ?
C3 Re1 C1 88.72(11) . . ?
Re1 O4 H4A 110(3) . . ?
Re1 O4 H4B 109(3) . . ?
H4A O4 H4B 111(4) . . ?
C9 O6 Re1 118.58(15) . . ?
C4 N1 Re1 126.04(15) . . ?
C4 N1 C8 118.7(2) . . ?
C8 N1 Re1 115.22(15) . . ?
O1 C1 Re1 179.4(3) . . ?
O2 C2 Re1 177.6(2) . . ?
O3 C3 Re1 175.6(2) . . ?
N1 C4 H4 119.3 . . ?
N1 C4 C5 121.4(2) . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C10 119.2(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 C10 120.9(2) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 C5 118.2(2) . . ?
C7 C6 H6 120.9 . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 119.0(2) . . ?
C8 C7 H7 120.5 . . ?
N1 C8 C7 122.9(2) . . ?
N1 C8 C9 115.6(2) . . ?
C7 C8 C9 121.5(2) . . ?
O5 C9 O6 125.5(2) . . ?
O5 C9 C8 119.2(2) . . ?
O6 C9 C8 115.3(2) . . ?
F1 C10 F2 106.2(2) . . ?
F1 C10 F3 107.9(2) . . ?
F1 C10 C5 112.3(2) . . ?
F2 C10 C5 111.9(2) . . ?
F3 C10 F2 106.1(2) . . ?
F3 C10 C5 112.0(2) . . ?
O12 Re2 O10 79.72(6) . . ?
O12 Re2 N2 75.34(7) . . ?
N2 Re2 O10 80.80(7) . . ?
C11 Re2 O10 95.45(9) . . ?
C11 Re2 O12 97.35(9) . . ?
C11 Re2 N2 172.23(10) . . ?
C12 Re2 O10 95.63(9) . . ?
C12 Re2 O12 171.76(9) . . ?
C12 Re2 N2 97.28(10) . . ?
C12 Re2 C11 89.83(12) . . ?
C12 Re2 C13 85.40(10) . . ?
C13 Re2 O10 176.20(9) . . ?
C13 Re2 O12 98.81(8) . . ?
C13 Re2 N2 95.45(10) . . ?
C13 Re2 C11 88.20(12) . . ?
Re2 O10 H10A 120(3) . . ?
Re2 O10 H10B 109(3) . . ?
H10A O10 H10B 111(4) . . ?
C19 O12 Re2 117.49(14) . . ?
C14 N2 Re2 127.34(16) . . ?
C14 N2 C18 117.8(2) . . ?
C18 N2 Re2 114.83(16) . . ?
O7 C11 Re2 179.3(3) . . ?
O8 C12 Re2 175.5(3) . . ?
O9 C13 Re2 176.0(2) . . ?
N2 C14 H14 119.0 . . ?
N2 C14 C15 122.0(2) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 C20 118.8(2) . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 C20 121.2(2) . . ?
C15 C16 H16 121.1 . . ?
C17 C16 C15 117.8(2) . . ?
C17 C16 H16 121.1 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.3(2) . . ?
C18 C17 H17 120.3 . . ?
N2 C18 C17 122.9(2) . . ?
N2 C18 C19 115.3(2) . . ?
C17 C18 C19 121.8(2) . . ?
O11 C19 O12 125.1(2) . . ?
O11 C19 C18 118.3(2) . . ?
O12 C19 C18 116.6(2) . . ?
F4 C20 C15 111.1(2) . . ?
F5 C20 F4 105.5(2) . . ?
F5 C20 C15 112.9(2) . . ?
F6 C20 F4 107.6(3) . . ?
F6 C20 F5 106.9(3) . . ?
F6 C20 C15 112.4(2) . . ?

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
O4 H4A O5 0.816(10) 1.842(11) 2.655(2) 174(4) 1_455 yes
O4 H4B O12 0.816(10) 1.952(12) 2.761(2) 171(4) 2_566 yes
O10 H10A O6 0.817(10) 1.883(13) 2.687(2) 168(4) 2_666 yes
O10 H10B O11 0.820(10) 1.818(11) 2.637(2) 177(4) 1_655 yes

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
Re1 O6 C9 O5 173.57(19) . . . . ?
Re1 O6 C9 C8 -6.8(3) . . . . ?
Re1 N1 C4 C5 175.88(18) . . . . ?
Re1 N1 C8 C7 -177.85(18) . . . . ?
Re1 N1 C8 C9 0.7(2) . . . . ?
N1 C4 C5 C6 1.6(4) . . . . ?
N1 C4 C5 C10 -177.9(2) . . . . ?
N1 C8 C9 O5 -176.4(2) . . . . ?
N1 C8 C9 O6 4.0(3) . . . . ?
C4 N1 C8 C7 -0.6(3) . . . . ?
C4 N1 C8 C9 177.9(2) . . . . ?
C4 C5 C6 C7 -0.5(4) . . . . ?
C4 C5 C10 F1 154.9(2) . . . . ?
C4 C5 C10 F2 -85.8(3) . . . . ?
C4 C5 C10 F3 33.3(3) . . . . ?
C5 C6 C7 C8 -1.1(4) . . . . ?
C6 C5 C10 F1 -24.6(4) . . . . ?
C6 C5 C10 F2 94.7(3) . . . . ?
C6 C5 C10 F3 -146.2(3) . . . . ?
C6 C7 C8 N1 1.7(4) . . . . ?
C6 C7 C8 C9 -176.7(2) . . . . ?
C7 C8 C9 O5 2.2(3) . . . . ?
C7 C8 C9 O6 -177.5(2) . . . . ?
C8 N1 C4 C5 -1.1(3) . . . . ?
C10 C5 C6 C7 179.1(2) . . . . ?
Re2 O12 C19 O11 173.53(18) . . . . ?
Re2 O12 C19 C18 -8.0(3) . . . . ?
Re2 N2 C14 C15 -178.58(17) . . . . ?
Re2 N2 C18 C17 177.28(18) . . . . ?
Re2 N2 C18 C19 -2.5(2) . . . . ?
N2 C14 C15 C16 1.1(4) . . . . ?
N2 C14 C15 C20 -178.3(2) . . . . ?
N2 C18 C19 O11 -174.4(2) . . . . ?
N2 C18 C19 O12 7.0(3) . . . . ?
C14 N2 C18 C17 -2.2(3) . . . . ?
C14 N2 C18 C19 178.0(2) . . . . ?
C14 C15 C16 C17 -1.8(4) . . . . ?
C14 C15 C20 F4 61.4(3) . . . . ?
C14 C15 C20 F5 179.8(2) . . . . ?
C14 C15 C20 F6 -59.3(4) . . . . ?
C15 C16 C17 C18 0.5(4) . . . . ?
C16 C15 C20 F4 -118.0(3) . . . . ?
C16 C15 C20 F5 0.4(4) . . . . ?
C16 C15 C20 F6 121.3(3) . . . . ?
C16 C17 C18 N2 1.6(4) . . . . ?
C16 C17 C18 C19 -178.7(2) . . . . ?
C17 C18 C19 O11 5.8(3) . . . . ?
C17 C18 C19 O12 -172.8(2) . . . . ?
C18 N2 C14 C15 0.8(3) . . . . ?
C20 C15 C16 C17 177.6(2) . . . . ?


####################################################################### 
# 
# 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_30
_database_code_depnum_ccdc_archive 'CCDC 2205515'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H7 N2 O6 Re, H2 O'
_chemical_formula_sum            'C9 H9 N2 O7 Re'
_chemical_formula_weight         443.38
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.23071(18)
_cell_length_b                   11.28656(8)
_cell_length_c                   8.98742(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.0757(8)
_cell_angle_gamma                90
_cell_volume                     2433.52(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      3.6650
_shelx_estimated_absorpt_T_max   0.182
_shelx_estimated_absorpt_T_min   0.043
_exptl_absorpt_coefficient_mu    19.885
_exptl_absorpt_correction_T_max  0.230
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0654
5 -2 -5 0.1513
5 4 -5 0.1316
-2 5 -1 0.0907
4 -5 -4 0.1539
-5 -4 5 0.0687
1 0 0 0.0654

_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13

_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11222
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.421
_diffrn_reflns_theta_min         3.685
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.00    --  -42.61 125.00  90.00   81
  2  ω   -129.00  44.00   1.00    1.00    --  -42.61   0.00 -30.00  173
  3  ω     11.00  42.00   1.00    1.00    --   42.61  78.00  65.23   31
  4  ω    103.00 178.00   1.00    3.00    --  111.00  77.00 120.00   75
  5  ω     30.00 107.00   1.00    3.00    --  111.00 -94.00  60.00   77
  6  ω    104.00 178.00   1.00    3.00    --  111.00 111.00  60.00   74
  7  ω     36.00 109.00   1.00    3.00    --  111.00-111.00-180.00   73
  8  ω     36.00 109.00   1.00    3.00    --  111.00-111.00-150.00   73
  9  ω    103.00 178.00   1.00    3.00    --  111.00  77.00  90.00   75
 10  ω    104.00 178.00   1.00    3.00    --  111.00 111.00 150.00   74
 11  ω     30.00 107.00   1.00    3.00    --  111.00 -94.00  90.00   77
 12  ω     36.00 109.00   1.00    3.00    --  111.00-111.00 -60.00   73
 13  ω    103.00 178.00   1.00    3.00    --  111.00  77.00 -30.00   75
 14  ω     61.00 146.00   1.00    3.00    --  111.00 178.00 150.00   85
 15  ω     30.00 107.00   1.00    3.00    --  111.00 -94.00-120.00   77
 16  ω    -65.00  30.00   1.00    1.00    --  -42.61  37.00  30.00   95
 17  ω     11.00  42.00   1.00    1.00    --   42.61  79.00  -3.84   31
 18  ω     16.00 113.00   1.00    1.00    --   42.61  57.00-120.00   97
 19  ω     10.00  42.00   1.00    1.00    --   42.61  80.00 168.78   32
 20  ω     87.00 178.00   1.00    3.00    --  111.00  30.00  60.00   91
 21  ω     87.00 172.00   1.00    3.00    --  111.00  30.00-150.00   85
 22  ω     87.00 178.00   1.00    3.00    --  111.00  45.00 -90.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057472000
_diffrn_orient_matrix_UB_12      0.0393567000
_diffrn_orient_matrix_UB_13      -0.1611609000
_diffrn_orient_matrix_UB_21      -0.0073376000
_diffrn_orient_matrix_UB_22      -0.1294746000
_diffrn_orient_matrix_UB_23      -0.0538242000
_diffrn_orient_matrix_UB_31      -0.0635323000
_diffrn_orient_matrix_UB_32      0.0185673000
_diffrn_orient_matrix_UB_33      -0.0329707000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2475
_reflns_number_total             2483

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       0.00082(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2483
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+8.6212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0706
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  H7 of C7, H6 of C6, H4 of C4
 At 1.5 times of:
  H7C of C2
2. Restrained distances
 O7-H7B = O7-H7A
 0.82 with sigma of 0.02
 O7-H7C
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.62799(17) 0.0021(4) 0.4270(5) 0.0203(8) Uani 1 1 d . . . . .
C2 C 0.6885(2) 0.1611(3) 0.5918(6) 0.0207(9) Uani 1 1 d . . . . .
H7C H 0.544(2) 0.055(3) 0.160(7) 0.031 Uiso 1 1 d D U . . .
C3 C 0.69338(17) 0.1401(4) 0.2952(5) 0.0217(8) Uani 1 1 d . . . . .
C4 C 0.66228(15) 0.4458(3) 0.4617(4) 0.0150(7) Uani 1 1 d . . . . .
H4 H 0.690542 0.419920 0.538879 0.018 Uiso 1 1 calc R U . . .
C5 C 0.65451(17) 0.5661(4) 0.4384(4) 0.0181(7) Uani 1 1 d . . . . .
C6 C 0.61331(17) 0.6048(3) 0.3225(5) 0.0187(7) Uani 1 1 d . . . . .
H6 H 0.607318 0.686841 0.302696 0.022 Uiso 1 1 calc R U . . .
C7 C 0.58183(17) 0.5200(4) 0.2383(4) 0.0176(8) Uani 1 1 d . . . . .
H7 H 0.553600 0.543287 0.159489 0.021 Uiso 1 1 calc R U . . .
C8 C 0.59148(15) 0.4006(3) 0.2688(4) 0.0134(7) Uani 1 1 d . . . . .
C9 C 0.55861(15) 0.3053(4) 0.1838(4) 0.0143(7) Uani 1 1 d . . . . .
N1 N 0.63146(12) 0.3643(3) 0.3794(4) 0.0138(6) Uani 1 1 d . . . . .
N2 N 0.68535(17) 0.6469(4) 0.5299(4) 0.0241(7) Uani 1 1 d . . . . .
H2A H 0.683(2) 0.713(6) 0.509(7) 0.027(15) Uiso 1 1 d . . . . .
H2B H 0.713(3) 0.616(6) 0.598(8) 0.048(18) Uiso 1 1 d . . . . .
O1 O 0.62539(15) -0.0981(3) 0.4319(4) 0.0319(7) Uani 1 1 d . . . . .
O2 O 0.71936(16) 0.1540(3) 0.6997(4) 0.0348(8) Uani 1 1 d . . . . .
O3 O 0.72752(14) 0.1164(3) 0.2248(4) 0.0309(7) Uani 1 1 d . . . . .
O4 O 0.56765(11) 0.2129(3) 0.5418(3) 0.0180(5) Uani 1 1 d . . . . .
H4A H 0.534(3) 0.248(6) 0.494(7) 0.040(16) Uiso 1 1 d . . . . .
H4B H 0.554(3) 0.149(7) 0.577(8) 0.043(19) Uiso 1 1 d . . . . .
O5 O 0.52174(14) 0.3304(2) 0.0801(4) 0.0199(7) Uani 1 1 d . . . . .
O6 O 0.57151(12) 0.1981(3) 0.2267(3) 0.0166(5) Uani 1 1 d . . . . .
O7 O 0.52990(14) -0.0111(3) 0.1359(4) 0.0261(6) Uani 1 1 d D . . . .
H7A H 0.514(9) -0.02(2) 0.049(10) 0.10(8) Uiso 0.5 1 d D . P A -2
H7B H 0.514(5) -0.023(10) 0.210(9) 0.03(3) Uiso 0.5 1 d D . P B -1
Re1 Re 0.63528(2) 0.17215(2) 0.41331(2) 0.01323(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.135(6) . ?
C1 Re1 1.932(5) . ?
C2 O2 1.141(6) . ?
C2 Re1 1.917(5) . ?
C3 O3 1.142(6) . ?
C3 Re1 1.913(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(6) . ?
C4 N1 1.340(5) . ?
C5 C6 1.407(6) . ?
C5 N2 1.376(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(5) . ?
C8 C9 1.485(5) . ?
C8 N1 1.350(5) . ?
C9 O5 1.230(5) . ?
C9 O6 1.296(5) . ?
N1 Re1 2.190(3) . ?
N2 H2A 0.77(7) . ?
N2 H2B 0.92(8) . ?
O4 H4A 0.96(7) . ?
O4 H4B 0.86(8) . ?
O4 Re1 2.182(3) . ?
O6 Re1 2.135(3) . ?
O7 H7C 0.83(2) . ?
O7 H7A 0.82(2) . ?
O7 H7B 0.83(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
O1 C1 Re1 177.3(4) . . ?
O2 C2 Re1 178.6(5) . . ?
O3 C3 Re1 177.3(4) . . ?
C5 C4 H4 118.7 . . ?
N1 C4 H4 118.7 . . ?
N1 C4 C5 122.5(4) . . ?
C4 C5 C6 119.0(4) . . ?
N2 C5 C4 120.6(4) . . ?
N2 C5 C6 120.4(4) . . ?
C5 C6 H6 121.0 . . ?
C7 C6 C5 118.0(4) . . ?
C7 C6 H6 121.0 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 122.5(3) . . ?
N1 C8 C7 121.6(3) . . ?
N1 C8 C9 115.9(3) . . ?
O5 C9 C8 120.3(4) . . ?
O5 C9 O6 124.0(4) . . ?
O6 C9 C8 115.7(3) . . ?
C4 N1 C8 119.0(3) . . ?
C4 N1 Re1 126.4(3) . . ?
C8 N1 Re1 114.5(3) . . ?
C5 N2 H2A 119(5) . . ?
C5 N2 H2B 116(5) . . ?
H2A N2 H2B 124(6) . . ?
H4A O4 H4B 100(6) . . ?
Re1 O4 H4A 121(4) . . ?
Re1 O4 H4B 111(5) . . ?
C9 O6 Re1 118.7(2) . . ?
H7C O7 H7A 116(10) . . ?
H7C O7 H7B 99(9) . . ?
C1 Re1 N1 171.74(15) . . ?
C1 Re1 O4 95.35(15) . . ?
C1 Re1 O6 97.09(14) . . ?
C2 Re1 C1 86.49(17) . . ?
C2 Re1 N1 101.04(15) . . ?
C2 Re1 O4 92.20(17) . . ?
C2 Re1 O6 173.97(15) . . ?
C3 Re1 C1 85.89(18) . . ?
C3 Re1 C2 89.5(2) . . ?
C3 Re1 N1 97.49(15) . . ?
C3 Re1 O4 177.99(14) . . ?
C3 Re1 O6 95.62(15) . . ?
O4 Re1 N1 81.07(11) . . ?
O6 Re1 N1 75.13(12) . . ?
O6 Re1 O4 82.66(11) . . ?

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
C4 C5 C6 C7 0.9(6) . . . . ?
C5 C4 N1 C8 0.4(6) . . . . ?
C5 C4 N1 Re1 -175.6(3) . . . . ?
C5 C6 C7 C8 -0.3(6) . . . . ?
C6 C7 C8 C9 179.2(4) . . . . ?
C6 C7 C8 N1 -0.4(6) . . . . ?
C7 C8 C9 O5 1.2(6) . . . . ?
C7 C8 C9 O6 -178.6(3) . . . . ?
C7 C8 N1 C4 0.3(5) . . . . ?
C7 C8 N1 Re1 176.8(3) . . . . ?
C8 C9 O6 Re1 1.5(4) . . . . ?
C9 C8 N1 C4 -179.3(3) . . . . ?
C9 C8 N1 Re1 -2.8(4) . . . . ?
N1 C4 C5 C6 -1.1(6) . . . . ?
N1 C4 C5 N2 177.0(4) . . . . ?
N1 C8 C9 O5 -179.3(4) . . . . ?
N1 C8 C9 O6 0.9(5) . . . . ?
N2 C5 C6 C7 -177.1(4) . . . . ?
O5 C9 O6 Re1 -178.2(3) . . . . ?


####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2205518'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;
_audit_creation_date             2021-07-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C9 H6 N O7 Re), H2 O'
_chemical_formula_sum            'C18 H14 N2 O15 Re2'
_chemical_formula_weight         870.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C18 H14 N2 O15 Re2'
_chemical_oxdiff_usercomment     3-OH
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8967(3)
_cell_length_b                   10.5952(3)
_cell_length_c                   12.8653(2)
_cell_angle_alpha                106.448(2)
_cell_angle_beta                 105.596(3)
_cell_angle_gamma                103.191(3)
_cell_volume                     1176.61(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23190
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      79.0560
_cell_measurement_theta_min      3.8280
_shelx_estimated_absorpt_T_max   0.233
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    20.556
_exptl_absorpt_correction_T_max  0.325
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             812
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -2 5 0.0606
-3 5 0 0.0606
-1 0 0 0.0406
-2 5 -5 0.0706
5 -2 1 0.0514
5 2 1 0.0527
1 1 -1 0.0639
5 -2 -2 0.0650
2 -5 0 0.0857
1 4 -5 0.0619
5 -4 -4 0.0652
1 -3 -5 0.0532
-3 1 5 0.0896

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0046 -2.0038 4.9945 0.1094 0.6352 -0.2261
-2.9847 4.9996 -0.0046 0.1254 -0.0120 0.7869
-1.0007 -0.0008 0.0019 0.1392 -0.0951 0.0300
-1.9948 5.0042 -4.9988 -0.1455 -0.5662 0.6743
4.9988 -1.9977 0.9931 -0.5528 0.4961 -0.4122
5.0128 2.0038 0.9848 -0.7865 0.7149 0.1453
1.0020 1.0019 -1.0024 -0.2240 0.0199 0.0929
4.9923 -1.9954 -2.0023 -0.6318 0.1065 -0.4618
1.9839 -5.0003 0.0065 0.0138 -0.0832 -0.7569
1.0038 4.0061 -5.0024 -0.5046 -0.3355 0.4449
4.9809 -3.9946 -3.9950 -0.5676 -0.2626 -0.7736
0.9793 -2.9965 -4.9879 -0.0956 -0.7183 -0.5308
-2.9878 0.9943 4.9959 0.4908 0.4187 0.3120

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21833
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.485
_diffrn_reflns_theta_min         3.835
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     87.00 177.00   0.50    0.20    --  107.75  77.00 -73.81  180
  2  ω    137.00 178.00   0.50    0.20    --  107.75  45.00 -60.00   82
  3  ω     96.00 132.00   0.50    0.20    --  107.75  45.00 -60.00   72
  4  ω     95.00 178.00   0.50    0.20    --  107.75  45.00 -90.00  166
  5  ω     94.00 169.00   0.50    0.20    --  107.75  30.00-120.00  150
  6  ω     92.00 151.00   0.50    0.20    --  107.75  61.00-180.00  118
  7  ω     32.00  87.00   0.50    0.20    --  107.75 -94.00-120.00  110
  8  ω     32.00 110.00   0.50    0.20    --  107.75-119.00-144.00  156
  9  ω     30.00  96.00   0.50    0.10    --   51.79-119.00-144.00  132
 10  ω     50.00 120.00   0.50    0.10    --   51.79-157.00  60.00  140
 11  ω     50.00 134.00   0.50    0.20    --  107.75-157.00  60.00  168
 12  ω     48.00  75.00   0.50    0.20    --  107.75-111.00 120.00   54
 13  ω     31.00 109.00   0.50    0.20    --  107.75-111.00 150.00  156
 14  ω     78.00 109.00   0.50    0.20    --  107.75-111.00  90.00   62
 15  ω     31.00  73.00   0.50    0.20    --  107.75-111.00  90.00   84
 16  ω     33.00 109.00   0.50    0.20    --  107.75-111.00  60.00  152
 17  ω     42.00  75.00   0.50    0.20    --  107.75-111.00   0.00   66
 18  ω     79.00 109.00   0.50    0.20    --  107.75-111.00   0.00   60
 19  ω     42.00 105.00   0.50    0.20    --  107.75-111.00 -60.00  126
 20  ω     32.00  71.00   0.50    0.20    --  107.75-111.00-120.00   78
 21  ω     76.00 109.00   0.50    0.20    --  107.75-111.00-120.00   66
 22  ω     48.00 108.00   0.50    0.20    --  107.75-111.00-180.00  120
 23  ω     29.00 112.00   0.50    0.20    --  107.75 -15.00 -60.00  166
 24  ω     37.00 124.00   0.50    0.20    --  107.75 -61.00-150.00  174
 25  ω     38.00 110.00   0.50    0.20    --  107.75 -61.00 -60.00  144
 26  ω     50.00 124.00   0.50    0.20    --  107.75 -61.00   0.00  148
 27  ω    100.00 126.00   0.50    0.20    --  107.75 -77.00 120.00   52
 28  ω     55.00  81.00   0.50    0.20    --  107.75 -77.00 120.00   52
 29  ω     30.00  96.00   0.50    0.20    --  107.75 -15.00  30.00  132
 30  ω    128.00 164.00   0.50    0.20    --  107.75 111.00-120.00   72
 31  ω     98.00 178.00   0.50    0.20    --  107.75 119.00 -58.00  160
 32  ω     72.00 126.00   0.50    0.10    --   51.79 157.00  96.00  108
 33  ω     72.00 161.00   0.50    0.20    --  107.75 157.00  96.00  178
 34  ω    -99.00 -10.00   0.50    0.20    --  -86.25  45.00 -30.00  178
 35  ω   -109.00 -28.00   0.50    0.10    --  -51.79 157.00  96.00  162
 36  ω    -84.00  -8.00   0.50    0.10    --  -51.79 119.00 -58.00  152
 37  ω    -85.00 -10.00   0.50    0.20    --  -86.25 119.00 -58.00  150
 38  ω   -124.00 -37.00   0.50    0.10    --  -51.79 -57.00-120.00  174
 39  ω   -125.00 -29.00   0.50    0.10    --  -51.79 -77.00   0.00  192
 40  ω   -125.00 -29.00   0.50    0.10    --  -51.79 -77.00 150.00  192
 41  ω   -144.00 -51.00   0.50    0.20    --  -86.25-157.00  60.00  186
 42  ω   -126.00 -51.00   0.50    0.10    --  -51.79-157.00  60.00  150
 43  ω   -162.00 -76.00   0.50    0.20    --  -86.25-119.00-144.00  172
 44  ω   -128.00 -76.00   0.50    0.10    --  -51.79-119.00-144.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1389995000
_diffrn_orient_matrix_UB_12      -0.0578753000
_diffrn_orient_matrix_UB_13      0.0266380000
_diffrn_orient_matrix_UB_21      0.0952634000
_diffrn_orient_matrix_UB_22      0.0545980000
_diffrn_orient_matrix_UB_23      0.1299151000
_diffrn_orient_matrix_UB_31      -0.0300521000
_diffrn_orient_matrix_UB_32      0.1394709000
_diffrn_orient_matrix_UB_33      0.0167282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4725
_reflns_number_total             4784
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00133(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4784
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0221
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0261P)²+3.0030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0565
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H) groups
2. Restrained distances
 O7-H7 = O4-H4B = O4-H4A = O11-H11A = O11-H11B = O14-H14A = O15-H15A = O15-H15B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.7334(5) 0.5270(4) 0.4974(3) 0.0247(8) Uani 1 1 d . . . . .
C2 C 0.6629(4) 0.3575(4) 0.6073(4) 0.0236(8) Uani 1 1 d . . . . .
C3 C 0.5456(5) 0.2706(4) 0.3797(4) 0.0240(8) Uani 1 1 d . . . . .
C4 C 0.7204(4) 0.0533(4) 0.5085(3) 0.0201(7) Uani 1 1 d . . . . .
H4 H 0.668829 0.078223 0.559418 0.024 Uiso 1 1 calc R U . . .
C5 C 0.7406(5) -0.0760(4) 0.4835(4) 0.0250(8) Uani 1 1 d . . . . .
H5 H 0.702089 -0.139374 0.516229 0.030 Uiso 1 1 calc R U . . .
C6 C 0.8172(5) -0.1115(4) 0.4107(4) 0.0240(8) Uani 1 1 d . . . . .
H6 H 0.831670 -0.199575 0.392921 0.029 Uiso 1 1 calc R U . . .
C7 C 0.8730(4) -0.0177(4) 0.3635(3) 0.0204(7) Uani 1 1 d . . . . .
C8 C 0.8467(4) 0.1098(4) 0.3907(3) 0.0160(7) Uani 1 1 d . . . . .
C9 C 0.8980(4) 0.2150(4) 0.3420(3) 0.0171(7) Uani 1 1 d . . . . .
C10 C 0.8726(5) 0.0943(4) -0.0844(4) 0.0270(9) Uani 1 1 d . . . . .
C11 C 0.7024(4) 0.0663(4) 0.0373(4) 0.0256(8) Uani 1 1 d . . . . .
H4A H 1.019(5) 0.4980(14) 0.632(4) 0.031 Uiso 1 1 d D U . . .
H4B H 0.986(6) 0.395(5) 0.664(3) 0.031 Uiso 1 1 d D U . . .
H7 H 0.969(6) 0.010(4) 0.269(4) 0.031 Uiso 1 1 d D U . . .
H11A H 0.990(6) 0.302(5) 0.183(4) 0.031 Uiso 1 1 d D U . . .
H11B H 1.034(4) 0.365(5) 0.120(5) 0.031 Uiso 1 1 d D U . . .
H14A H 0.740(5) 0.701(6) 0.037(3) 0.031 Uiso 1 1 d D U . . .
H15A H 0.984(6) 0.235(4) -0.234(5) 0.038 Uiso 1 1 d D U . . .
H15B H 0.924(6) 0.326(6) -0.191(4) 0.038 Uiso 1 1 d D U . . .
C12 C 0.5995(5) 0.1123(4) -0.1589(4) 0.0281(9) Uani 1 1 d . . . . .
C13 C 0.5954(4) 0.3403(4) 0.1314(4) 0.0237(8) Uani 1 1 d . . . . .
H13 H 0.568614 0.253626 0.141273 0.028 Uiso 1 1 calc R U . . .
C14 C 0.5511(4) 0.4478(5) 0.1872(4) 0.0253(8) Uani 1 1 d . . . . .
H14 H 0.495008 0.433825 0.234797 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5874(5) 0.5731(5) 0.1741(3) 0.0255(8) Uani 1 1 d . . . . .
H15 H 0.557637 0.646661 0.212410 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6694(4) 0.5911(4) 0.1030(3) 0.0214(8) Uani 1 1 d . . . . .
C17 C 0.7112(4) 0.4791(4) 0.0486(3) 0.0177(7) Uani 1 1 d . . . . .
C18 C 0.7986(4) 0.4884(4) -0.0278(3) 0.0194(7) Uani 1 1 d . . . . .
N1 N 0.7723(3) 0.1436(3) 0.4621(3) 0.0157(6) Uani 1 1 d . . . . .
N2 N 0.6751(3) 0.3569(3) 0.0640(3) 0.0172(6) Uani 1 1 d . . . . .
O1 O 0.7204(4) 0.6328(3) 0.4985(3) 0.0384(8) Uani 1 1 d . . . . .
O2 O 0.6141(4) 0.3600(4) 0.6788(3) 0.0382(8) Uani 1 1 d . . . . .
O3 O 0.4259(4) 0.2252(4) 0.3151(3) 0.0388(8) Uani 1 1 d . . . . .
O4 O 0.9767(3) 0.4133(3) 0.6049(2) 0.0192(5) Uani 1 1 d D . . . .
O5 O 0.9727(3) 0.1930(3) 0.2789(2) 0.0222(5) Uani 1 1 d . . . . .
O6 O 0.8581(3) 0.3240(3) 0.3661(2) 0.0189(5) Uani 1 1 d . . . . .
O7 O 0.9504(3) -0.0513(3) 0.2949(3) 0.0258(6) Uani 1 1 d D . . . .
O8 O 0.9333(5) 0.0241(4) -0.1224(4) 0.0484(10) Uani 1 1 d . . . . .
O9 O 0.6579(4) -0.0188(4) 0.0700(3) 0.0416(8) Uani 1 1 d . . . . .
O10 O 0.5014(4) 0.0577(4) -0.2441(3) 0.0453(9) Uani 1 1 d . . . . .
O11 O 0.9621(3) 0.3400(3) 0.1381(2) 0.0203(5) Uani 1 1 d D . . . .
O12 O 0.8279(3) 0.5970(3) -0.0509(3) 0.0242(6) Uani 1 1 d . . . . .
O13 O 0.8385(3) 0.3837(3) -0.0665(2) 0.0199(5) Uani 1 1 d . . . . .
O14 O 0.7019(3) 0.7119(3) 0.0871(3) 0.0293(6) Uani 1 1 d D . . . .
O15 O 0.9641(4) 0.3045(3) -0.2380(3) 0.0297(6) Uani 1 1 d D . . . .
Re1 Re 0.74502(2) 0.34642(2) 0.48805(2) 0.01597(7) Uani 1 1 d . . . . .
Re2 Re 0.76832(2) 0.20794(2) -0.01892(2) 0.01687(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
C1 O1 1.154(5) . ?
C1 Re1 1.914(4) . ?
C2 O2 1.145(5) . ?
C2 Re1 1.908(4) . ?
C3 O3 1.145(5) . ?
C3 Re1 1.909(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(5) . ?
C4 N1 1.342(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(6) . ?
C7 C8 1.398(5) . ?
C7 O7 1.343(5) . ?
C8 C9 1.484(5) . ?
C8 N1 1.346(5) . ?
C9 O5 1.246(5) . ?
C9 O6 1.288(4) . ?
C10 O8 1.143(5) . ?
C10 Re2 1.920(4) . ?
C11 O9 1.147(6) . ?
C11 Re2 1.903(4) . ?
C12 O10 1.137(5) . ?
C12 Re2 1.907(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.393(6) . ?
C13 N2 1.339(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.364(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.399(6) . ?
C16 C17 1.406(5) . ?
C16 O14 1.334(5) . ?
C17 C18 1.483(5) . ?
C17 N2 1.348(5) . ?
C18 O12 1.259(5) . ?
C18 O13 1.276(5) . ?
N1 Re1 2.170(3) . ?
N2 Re2 2.173(3) . ?
O4 H4A 0.821(10) . ?
O4 H4B 0.821(10) . ?
O4 Re1 2.196(3) . ?
O6 Re1 2.150(3) . ?
O7 H7 0.820(10) . ?
O11 H11A 0.821(10) . ?
O11 H11B 0.819(10) . ?
O11 Re2 2.193(3) . ?
O13 Re2 2.147(3) . ?
O14 H14A 0.821(10) . ?
O15 H15A 0.817(10) . ?
O15 H15B 0.819(10) . ?

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
O1 C1 Re1 176.8(4) . . ?
O2 C2 Re1 177.7(4) . . ?
O3 C3 Re1 179.7(4) . . ?
C5 C4 H4 119.4 . . ?
N1 C4 H4 119.4 . . ?
N1 C4 C5 121.3(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.3(4) . . ?
C6 C5 H5 120.3 . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.7(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 118.1(4) . . ?
O7 C7 C6 119.5(3) . . ?
O7 C7 C8 122.5(4) . . ?
C7 C8 C9 122.1(3) . . ?
N1 C8 C7 121.8(3) . . ?
N1 C8 C9 116.1(3) . . ?
O5 C9 C8 119.6(3) . . ?
O5 C9 O6 123.7(3) . . ?
O6 C9 C8 116.6(3) . . ?
O8 C10 Re2 178.3(4) . . ?
O9 C11 Re2 177.7(4) . . ?
O10 C12 Re2 177.7(4) . . ?
C14 C13 H13 119.4 . . ?
N2 C13 H13 119.4 . . ?
N2 C13 C14 121.2(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 120.7 . . ?
C14 C15 C16 118.6(4) . . ?
C16 C15 H15 120.7 . . ?
C15 C16 C17 118.4(4) . . ?
O14 C16 C15 119.1(4) . . ?
O14 C16 C17 122.5(4) . . ?
C16 C17 C18 122.3(3) . . ?
N2 C17 C16 121.7(3) . . ?
N2 C17 C18 115.9(3) . . ?
O12 C18 C17 118.7(3) . . ?
O12 C18 O13 124.3(4) . . ?
O13 C18 C17 117.0(3) . . ?
C4 N1 C8 119.8(3) . . ?
C4 N1 Re1 126.0(3) . . ?
C8 N1 Re1 114.2(2) . . ?
C13 N2 C17 119.4(3) . . ?
C13 N2 Re2 126.5(3) . . ?
C17 N2 Re2 114.0(2) . . ?
H4A O4 H4B 103(5) . . ?
Re1 O4 H4A 114(4) . . ?
Re1 O4 H4B 113(4) . . ?
C9 O6 Re1 116.7(2) . . ?
C7 O7 H7 109(4) . . ?
H11A O11 H11B 104(5) . . ?
Re2 O11 H11A 116(4) . . ?
Re2 O11 H11B 109(4) . . ?
C18 O13 Re2 117.2(2) . . ?
C16 O14 H14A 106(4) . . ?
H15A O15 H15B 108(6) . . ?
C1 Re1 N1 172.79(15) . . ?
C1 Re1 O4 97.87(14) . . ?
C1 Re1 O6 96.88(14) . . ?
C2 Re1 C1 88.45(17) . . ?
C2 Re1 C3 87.16(17) . . ?
C2 Re1 N1 98.73(14) . . ?
C2 Re1 O4 95.19(14) . . ?
C2 Re1 O6 172.47(13) . . ?
C3 Re1 C1 87.39(17) . . ?
C3 Re1 N1 93.60(14) . . ?
C3 Re1 O4 174.29(13) . . ?
C3 Re1 O6 98.36(14) . . ?
N1 Re1 O4 80.90(11) . . ?
O6 Re1 N1 75.91(10) . . ?
O6 Re1 O4 78.85(10) . . ?
C10 Re2 N2 173.20(16) . . ?
C10 Re2 O11 94.27(15) . . ?
C10 Re2 O13 99.72(14) . . ?
C11 Re2 C10 86.24(18) . . ?
C11 Re2 C12 89.43(18) . . ?
C11 Re2 N2 98.04(15) . . ?
C11 Re2 O11 96.48(14) . . ?
C11 Re2 O13 173.46(15) . . ?
C12 Re2 C10 89.08(19) . . ?
C12 Re2 N2 96.21(15) . . ?
C12 Re2 O11 173.37(14) . . ?
C12 Re2 O13 93.34(15) . . ?
N2 Re2 O11 80.04(11) . . ?
O13 Re2 N2 75.78(11) . . ?
O13 Re2 O11 80.47(10) . . ?

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
C5 H5 O1 0.95 2.41 3.110(5) 130.0 1_545 yes
O4 H4A O6 0.821(10) 1.99(3) 2.750(4) 155(5) 2_766 yes
O4 H4B O15 0.821(10) 1.816(19) 2.612(4) 163(5) 1_556 yes
O7 H7 O5 0.820(10) 1.90(3) 2.618(4) 146(5) . yes
O11 H11A O5 0.821(10) 1.92(2) 2.700(4) 158(5) . yes
O11 H11B O12 0.819(10) 1.848(15) 2.659(4) 170(5) 2_765 yes
O14 H14A O12 0.821(10) 1.88(3) 2.617(4) 150(5) . yes
O15 H15A O7 0.817(10) 2.19(3) 2.950(4) 155(6) 2_755 yes
O15 H15B O13 0.819(10) 2.014(12) 2.831(4) 176(6) . yes
C15 H15 O2 0.95 2.48 3.159(5) 128.7 2_666 yes

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
C4 C5 C6 C7 0.0(6) . . . . ?
C5 C4 N1 C8 -0.6(6) . . . . ?
C5 C4 N1 Re1 178.1(3) . . . . ?
C5 C6 C7 C8 -1.1(6) . . . . ?
C5 C6 C7 O7 178.5(4) . . . . ?
C6 C7 C8 C9 -178.2(3) . . . . ?
C6 C7 C8 N1 1.3(6) . . . . ?
C7 C8 C9 O5 -3.3(5) . . . . ?
C7 C8 C9 O6 175.0(3) . . . . ?
C7 C8 N1 C4 -0.5(5) . . . . ?
C7 C8 N1 Re1 -179.4(3) . . . . ?
C8 C9 O6 Re1 6.6(4) . . . . ?
C9 C8 N1 C4 179.1(3) . . . . ?
C9 C8 N1 Re1 0.2(4) . . . . ?
C13 C14 C15 C16 0.3(6) . . . . ?
C14 C13 N2 C17 -1.0(6) . . . . ?
C14 C13 N2 Re2 175.0(3) . . . . ?
C14 C15 C16 C17 -0.3(6) . . . . ?
C14 C15 C16 O14 178.2(4) . . . . ?
C15 C16 C17 C18 -179.7(3) . . . . ?
C15 C16 C17 N2 -0.4(5) . . . . ?
C16 C17 C18 O12 -4.9(5) . . . . ?
C16 C17 C18 O13 175.6(3) . . . . ?
C16 C17 N2 C13 1.1(5) . . . . ?
C16 C17 N2 Re2 -175.4(3) . . . . ?
C17 C18 O13 Re2 1.5(4) . . . . ?
C18 C17 N2 C13 -179.6(3) . . . . ?
C18 C17 N2 Re2 3.9(4) . . . . ?
N1 C4 C5 C6 0.8(6) . . . . ?
N1 C8 C9 O5 177.1(3) . . . . ?
N1 C8 C9 O6 -4.6(5) . . . . ?
N2 C13 C14 C15 0.3(6) . . . . ?
N2 C17 C18 O12 175.8(3) . . . . ?
N2 C17 C18 O13 -3.7(5) . . . . ?
O5 C9 O6 Re1 -175.2(3) . . . . ?
O7 C7 C8 C9 2.2(6) . . . . ?
O7 C7 C8 N1 -178.2(3) . . . . ?
O12 C18 O13 Re2 -178.0(3) . . . . ?
O14 C16 C17 C18 1.9(6) . . . . ?
O14 C16 C17 N2 -178.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.495
_oxdiff_exptl_absorpt_empirical_full_min 0.707
####################################################################### 
# 
# 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_31
_database_code_depnum_ccdc_archive 'CCDC 2205520'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 N2 O8 Re, H2 O'
_chemical_formula_sum            'C9 H7 N2 O9 Re'
_chemical_formula_weight         473.37
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   6.46680(10)
_cell_length_b                   24.4678(3)
_cell_length_c                   8.21830(10)
_cell_angle_alpha                90
_cell_angle_beta                 102.6050(10)
_cell_angle_gamma                90
_cell_volume                     1269.03(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12683
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.7230
_cell_measurement_theta_min      3.6140
_shelx_estimated_absorpt_T_max   0.308
_shelx_estimated_absorpt_T_min   0.053
_exptl_absorpt_coefficient_mu    19.257
_exptl_absorpt_correction_T_max  0.365
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0274
0 1 0 0.0504
0 -1 1 0.0451
0 1 -1 0.0341
-1 -1 1 0.1419
1 1 -1 0.1419
0 -5 -2 0.0350
0 5 2 0.0540
-4 1 1 0.1748

_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08

_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_min         3.613
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     86.00 178.00   0.50    0.20    --  107.75  76.00  39.00  184
  2  ω    104.00 132.00   0.50    0.20    --  107.75 111.00 -90.00   56
  3  ω    140.00 165.00   0.50    0.20    --  107.75 111.00 -90.00   50
  4  ω     95.00 178.00   0.50    0.20    --  107.75  45.00   0.00  166
  5  ω   -125.00 -30.00   0.50    0.10    --  -51.79 -76.00 -87.00  190
  6  ω   -126.00 -73.00   0.50    0.10    --  -51.79-125.00   0.00  106
  7  ω   -159.00 -64.00   0.50    0.20    --  -86.25 -76.00 -87.00  190
  8  ω    -21.00  74.00   0.50    0.10    --   51.79 -76.00 -87.00  190
  9  ω     34.00 130.00   0.50    0.20    --  107.75 -77.00 -30.00  192
 10  ω     35.00 130.00   0.50    0.20    --  107.75 -76.00 -87.00  190
 11  ω     28.00 120.00   0.50    0.20    --  107.75 -15.00-120.00  184
 12  ω     32.00 120.00   0.50    0.20    --  107.75 -45.00 -30.00  176
 13  ω     29.00 112.00   0.50    0.20    --  107.75 -15.00  30.00  166
 14  ω     30.00  93.00   0.50    0.20    --  107.75 -30.00 120.00  126
 15  ω    -74.00  21.00   0.50    0.10    --  -51.79  76.00  39.00  190
 16  ω   -108.00 -13.00   0.50    0.20    --  -86.25  76.00  39.00  190
 17  ω    -83.00  -9.00   0.50    0.20    --  -86.25 111.00 150.00  148
 18  ω     42.00  95.00   0.50    0.20    --  107.75 -94.00 120.00  106
 19  ω     36.00  87.00   0.50    0.20    --  107.75 -94.00 -90.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0840645000
_diffrn_orient_matrix_UB_12      0.0476466000
_diffrn_orient_matrix_UB_13      -0.1185332000
_diffrn_orient_matrix_UB_21      0.1257028000
_diffrn_orient_matrix_UB_22      -0.0215581000
_diffrn_orient_matrix_UB_23      -0.1257551000
_diffrn_orient_matrix_UB_31      -0.1916944000
_diffrn_orient_matrix_UB_32      -0.0350393000
_diffrn_orient_matrix_UB_33      -0.0838954000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2566
_reflns_number_total             2590

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.00431(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2590
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.257
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0436P)²+2.2662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0777
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4A = O9-H9A = O9-H9B
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.10183(3) 0.58351(2) 0.34351(2) 0.01724(12) Uani 1 1 d . . . . .
O1 O -0.1752(5) 0.50479(14) 0.0970(4) 0.0278(7) Uani 1 1 d . . . . .
O2 O 0.4291(7) 0.58675(14) 0.1264(5) 0.0332(9) Uani 1 1 d . . . . .
O3 O -0.1292(7) 0.67793(16) 0.1384(5) 0.0404(10) Uani 1 1 d . . . . .
O4 O 0.2660(6) 0.51996(13) 0.5061(4) 0.0244(7) Uani 1 1 d D . . . .
O5 O 0.8136(5) 0.71661(14) 0.5538(4) 0.0307(7) Uani 1 1 d . . . . .
O6 O 0.8125(7) 0.75340(17) 0.7928(6) 0.0447(10) Uani 1 1 d . . . . .
O7 O -0.1059(5) 0.60736(13) 0.7862(4) 0.0261(7) Uani 1 1 d . . . . .
O8 O -0.0895(6) 0.58197(11) 0.5280(5) 0.0227(7) Uani 1 1 d . . . . .
O9 O 0.5328(5) 0.54813(15) 0.7763(4) 0.0288(7) Uani 1 1 d D . . . .
H9A H 0.534(11) 0.542(3) 0.874(3) 0.043 Uiso 1 1 d D U . . .
H4A H 0.237(11) 0.4875(8) 0.493(9) 0.043 Uiso 1 1 d D U . . .
N1 N 0.2697(6) 0.63572(14) 0.5436(4) 0.0178(7) Uani 1 1 d . . . . .
N2 N 0.7361(6) 0.72356(15) 0.6754(5) 0.0248(8) Uani 1 1 d . . . . .
C1 C -0.0684(7) 0.5336(2) 0.1874(6) 0.0232(9) Uani 1 1 d . . . . .
C2 C 0.3036(9) 0.58512(16) 0.2049(7) 0.0238(11) Uani 1 1 d . . . . .
H4B H 0.377(10) 0.521(3) 0.592(9) 0.036 Uiso 1 1 d . U . . .
H9B H 0.643(6) 0.562(2) 0.761(8) 0.036 Uiso 1 1 d D U . . .
C3 C -0.0433(8) 0.6423(2) 0.2152(6) 0.0282(10) Uani 1 1 d . . . . .
C4 C 0.4506(7) 0.66248(16) 0.5460(5) 0.0182(8) Uani 1 1 d . . . . .
H4 H 0.517013 0.659676 0.454027 0.022 Uiso 1 1 calc R U . . .
C5 C 0.5405(7) 0.69406(16) 0.6813(5) 0.0201(8) Uani 1 1 d . . . . .
C6 C 0.4532(7) 0.69875(18) 0.8198(5) 0.0239(9) Uani 1 1 d . . . . .
H6 H 0.518001 0.720273 0.913225 0.029 Uiso 1 1 calc R U . . .
C7 C 0.2667(7) 0.67052(18) 0.8156(5) 0.0230(9) Uani 1 1 d . . . . .
H7 H 0.198552 0.672531 0.906755 0.028 Uiso 1 1 calc R U . . .
C8 C 0.1812(6) 0.63949(16) 0.6775(5) 0.0181(8) Uani 1 1 d . . . . .
C9 C -0.0210(7) 0.60719(16) 0.6661(5) 0.0199(8) 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 O4 2.171(3) . ?
Re1 O8 2.156(4) . ?
Re1 N1 2.176(3) . ?
Re1 C1 1.932(5) . ?
Re1 C2 1.911(6) . ?
Re1 C3 1.905(5) . ?
O1 C1 1.141(6) . ?
O2 C2 1.142(7) . ?
O3 C3 1.146(7) . ?
O4 H4A 0.819(10) . ?
O4 H4B 0.89(7) . ?
O5 N2 1.223(5) . ?
O6 N2 1.225(6) . ?
O7 C9 1.229(5) . ?
O8 C9 1.283(5) . ?
O9 H9A 0.817(10) . ?
O9 H9B 0.819(10) . ?
N1 C4 1.337(6) . ?
N1 C8 1.349(5) . ?
N2 C5 1.466(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.375(6) . ?
C5 C6 1.381(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C8 C9 1.513(6) . ?

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
O4 Re1 N1 81.89(12) . . ?
O8 Re1 O4 80.40(13) . . ?
O8 Re1 N1 75.35(13) . . ?
C1 Re1 O4 95.01(17) . . ?
C1 Re1 O8 97.16(16) . . ?
C1 Re1 N1 172.24(16) . . ?
C2 Re1 O4 94.35(18) . . ?
C2 Re1 O8 172.26(18) . . ?
C2 Re1 N1 98.38(18) . . ?
C2 Re1 C1 88.9(2) . . ?
C3 Re1 O4 175.78(16) . . ?
C3 Re1 O8 96.52(18) . . ?
C3 Re1 N1 94.56(16) . . ?
C3 Re1 C1 88.2(2) . . ?
C3 Re1 C2 88.4(2) . . ?
Re1 O4 H4A 123(5) . . ?
Re1 O4 H4B 132(4) . . ?
H4A O4 H4B 104(7) . . ?
C9 O8 Re1 118.3(3) . . ?
H9A O9 H9B 113(7) . . ?
C4 N1 Re1 126.1(3) . . ?
C4 N1 C8 118.7(4) . . ?
C8 N1 Re1 115.2(3) . . ?
O5 N2 O6 124.0(4) . . ?
O5 N2 C5 118.0(4) . . ?
O6 N2 C5 118.0(4) . . ?
O1 C1 Re1 177.5(4) . . ?
O2 C2 Re1 177.7(5) . . ?
O3 C3 Re1 179.4(5) . . ?
N1 C4 H4 119.9 . . ?
N1 C4 C5 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 N2 117.7(4) . . ?
C4 C5 C6 122.4(4) . . ?
C6 C5 N2 119.8(4) . . ?
C5 C6 H6 121.7 . . ?
C5 C6 C7 116.7(4) . . ?
C7 C6 H6 121.7 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.1(4) . . ?
C8 C7 H7 120.4 . . ?
N1 C8 C7 123.0(4) . . ?
N1 C8 C9 115.4(3) . . ?
C7 C8 C9 121.7(4) . . ?
O7 C9 O8 125.7(4) . . ?
O7 C9 C8 118.7(4) . . ?
O8 C9 C8 115.6(4) . . ?

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
O4 H4A O8 0.819(10) 1.94(2) 2.732(4) 163(7) 3_566 yes
O4 H4B O9 0.89(7) 1.76(7) 2.590(5) 155(6) . yes
O9 H9B O7 0.819(10) 1.94(2) 2.736(5) 162(7) 1_655 yes

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
Re1 O8 C9 O7 -175.6(3) . . . . ?
Re1 O8 C9 C8 4.9(5) . . . . ?
Re1 N1 C4 C5 -179.7(3) . . . . ?
Re1 N1 C8 C7 179.7(3) . . . . ?
Re1 N1 C8 C9 -0.4(4) . . . . ?
O5 N2 C5 C4 -3.2(6) . . . . ?
O5 N2 C5 C6 177.0(4) . . . . ?
O6 N2 C5 C4 177.3(4) . . . . ?
O6 N2 C5 C6 -2.6(6) . . . . ?
N1 C4 C5 N2 -178.5(3) . . . . ?
N1 C4 C5 C6 1.3(6) . . . . ?
N1 C8 C9 O7 177.5(4) . . . . ?
N1 C8 C9 O8 -2.9(5) . . . . ?
N2 C5 C6 C7 178.9(4) . . . . ?
C4 N1 C8 C7 1.2(6) . . . . ?
C4 N1 C8 C9 -178.9(3) . . . . ?
C4 C5 C6 C7 -0.9(6) . . . . ?
C5 C6 C7 C8 0.7(6) . . . . ?
C6 C7 C8 N1 -0.9(6) . . . . ?
C6 C7 C8 C9 179.3(4) . . . . ?
C7 C8 C9 O7 -2.6(6) . . . . ?
C7 C8 C9 O8 176.9(4) . . . . ?
C8 N1 C4 C5 -1.4(6) . . . . ?


####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 2205521'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-07-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C9 H7 N2 O6 Re), H2 O'
_chemical_formula_sum            'C18 H16 N4 O13 Re2'
_chemical_formula_weight         868.75
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5868(2)
_cell_length_b                   13.4770(3)
_cell_length_c                   18.0923(3)
_cell_angle_alpha                82.284(2)
_cell_angle_beta                 87.5270(10)
_cell_angle_gamma                68.815(2)
_cell_volume                     2385.09(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    36172
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      73.3710
_cell_measurement_theta_min      2.4360
_shelx_estimated_absorpt_T_max   0.688
_shelx_estimated_absorpt_T_min   0.195
_exptl_absorpt_coefficient_mu    20.238
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.0168
0 1 -1 0.0078
1 -3 -5 0.0493
5 2 -1 0.0314
-5 -4 -1 0.0440
2 -4 -5 0.0464
2 5 4 0.0346
-4 2 5 0.0381

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02

_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44910
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.370
_diffrn_reflns_theta_min         2.465
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -7.00   0.80    3.00    --  -42.74 125.00 -60.00  100
  2  ω   -121.00  -6.60   0.80    3.00    --  -42.74 -19.00-150.00  143
  3  ω   -116.00 -20.00   0.80    3.00    --  -42.74 -37.00 120.00  120
  4  ω     11.00  40.60   0.80    3.00    --   42.74  78.00 103.63   37
  5  ω     27.00  97.40   0.80    3.00    --   42.74-125.00 -60.00   88
  6  ω     81.00 177.00   0.80   10.00    --  104.82  30.00  30.00  120
  7  ω    103.00 177.40   0.80   10.00    --  104.82  77.00  60.00   93
  8  ω     34.00 128.40   0.80   10.00    --  104.82 -45.00 -30.00  118
  9  ω     35.00 131.00   0.80   10.00    --  104.82 -61.00-180.00  120
 10  ω     33.00 113.00   0.80   10.00    --  104.82-125.00-150.00  100
 11  ω     97.00 175.40   0.80   10.00    --  104.82 125.00-120.00   98
 12  ω    103.00 177.40   0.80   10.00    --  104.82  77.00 -90.00   93
 13  ω     33.00 113.00   0.80   10.00    --  104.82-125.00 120.00  100
 14  ω     24.00 105.60   0.80   10.00    --  104.82 -94.00   0.00  102
 15  ω     24.00 105.60   0.80   10.00    --  104.82 -94.00 -60.00  102
 16  ω     75.00 176.60   0.80   10.00    --  104.82  71.00 -44.65  127
 17  ω    102.00 178.00   0.80   10.00    --  104.82 115.00 -11.00   95
 18  ω     28.00 108.00   0.80   10.00    --  104.82-105.00 -93.48  100
 19  ω   -113.00 -17.00   0.80    3.00    --  -42.74 -57.00  30.00  120
 20  ω    -69.00  27.00   0.80    3.00    --  -42.74  57.00-180.00  120
 21  ω     11.00  40.60   0.80    3.00    --   42.74  80.00 -39.63   37
 22  ω     11.00  40.60   0.80    3.00    --   42.74  79.00-104.34   37
 23  ω     10.00  42.00   0.80    3.00    --   42.74  81.00   1.19   40
 24  ω     81.00 177.00   0.80   10.00    --  104.82  30.00-120.00  120
 25  ω     77.00 174.60   0.80   10.00    --  104.82  61.00-120.00  122
 26  ω     81.00 177.00   0.80   10.00    --  104.82  30.00 150.00  120
 27  ω     77.00 174.60   0.80   10.00    --  104.82  63.00  39.45  122
 28  ω     75.00 175.00   0.80   10.00    --  104.82  69.00 -85.85  125
 29  ω     78.00 174.00   0.80   10.00    --  104.82  59.00 171.99  120
 30  ω     75.00 175.00   0.80   10.00    --  104.82  69.00 132.03  125
 31  ω     76.00 174.40   0.80   10.00    --  104.82  65.00  10.88  123
 32  ω     76.00 174.40   0.80   10.00    --  104.82  65.00 104.49  123
 33  ω     75.00 175.00   0.80   10.00    --  104.82  69.00  74.84  125
 34  ω     13.00 107.40   0.80    3.00    --   42.74  70.00 173.14  118
 35  ω     11.00  40.60   0.80    3.00    --   42.74  77.00  41.23   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0324722000
_diffrn_orient_matrix_UB_12      -0.0945496000
_diffrn_orient_matrix_UB_13      -0.0458694000
_diffrn_orient_matrix_UB_21      0.0512674000
_diffrn_orient_matrix_UB_22      -0.0795957000
_diffrn_orient_matrix_UB_23      0.0712039000
_diffrn_orient_matrix_UB_31      -0.1437841000
_diffrn_orient_matrix_UB_32      -0.0015478000
_diffrn_orient_matrix_UB_33      0.0144863000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9333
_reflns_number_total             9457

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.000064(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         9457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0150
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0148P)²+2.6749P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0355
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23),
 C24(H24), C31(H31), C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.4577(3) 0.3790(2) 0.12389(16) 0.0303(6) Uani 1 1 d . . . . .
C2 C 0.6294(3) 0.4042(2) 0.21466(15) 0.0273(6) Uani 1 1 d . . . . .
C3 C 0.7017(3) 0.2282(2) 0.14546(15) 0.0275(6) Uani 1 1 d . . . . .
C4 C 0.9240(3) 0.3875(2) 0.13946(14) 0.0215(5) Uani 1 1 d . . . . .
H4 H 0.894649 0.394422 0.189501 0.026 Uiso 1 1 calc R U . . .
C5 C 1.0533(3) 0.3852(2) 0.11991(16) 0.0260(5) Uani 1 1 d . . . . .
H5 H 1.111285 0.391624 0.156128 0.031 Uiso 1 1 calc R U . . .
C6 C 1.0965(3) 0.3736(2) 0.04805(16) 0.0264(5) Uani 1 1 d . . . . .
H6 H 1.185224 0.371171 0.034579 0.032 Uiso 1 1 calc R U . . .
C7 C 1.0101(3) 0.36518(19) -0.00609(15) 0.0229(5) Uani 1 1 d . . . . .
C8 C 0.8798(3) 0.37024(19) 0.01728(14) 0.0198(5) Uani 1 1 d . . . . .
C9 C 0.7751(3) 0.36675(19) -0.03359(14) 0.0204(5) Uani 1 1 d . . . . .
C10 C 0.8901(3) 0.6630(3) 0.28653(16) 0.0321(6) Uani 1 1 d . . . . .
H2A H 0.993(4) 0.355(3) -0.110(2) 0.048 Uiso 1 1 d . U . . .
H2B H 1.120(4) 0.366(3) -0.089(2) 0.048 Uiso 1 1 d . U . . .
H4C H 0.218(4) 0.644(3) 0.483(2) 0.048 Uiso 1 1 d . U . . .
H4D H 0.269(4) 0.651(3) 0.404(2) 0.048 Uiso 1 1 d . U . . .
H6A H 0.711(4) 0.899(3) 0.156(2) 0.048 Uiso 1 1 d . U . . .
H6B H 0.789(4) 0.871(3) 0.090(2) 0.048 Uiso 1 1 d . U . . .
H8A H -0.014(4) 0.107(3) 0.579(2) 0.048 Uiso 1 1 d . U . . .
H8B H -0.149(4) 0.114(3) 0.562(2) 0.048 Uiso 1 1 d . U . . .
H4A H 0.597(4) 0.580(3) 0.096(2) 0.048 Uiso 1 1 d . U . . .
H4B H 0.511(5) 0.575(3) 0.052(2) 0.048 Uiso 1 1 d . U . . .
H10A H 0.643(4) 0.847(3) 0.330(3) 0.048 Uiso 1 1 d . U . . .
H10B H 0.704(4) 0.846(3) 0.389(2) 0.048 Uiso 1 1 d . U . . .
H16A H 0.290(4) 0.691(3) 0.161(2) 0.048 Uiso 1 1 d . U . . .
H16B H 0.346(4) 0.704(3) 0.225(2) 0.048 Uiso 1 1 d . U . . .
H22A H 0.377(4) -0.051(3) 0.398(2) 0.048 Uiso 1 1 d . U . . .
H22B H 0.346(4) -0.049(3) 0.328(2) 0.048 Uiso 1 1 d . U . . .
H25A H 0.641(4) 0.643(3) 0.208(2) 0.048 Uiso 1 1 d . U . . .
H25B H 0.685(4) 0.692(4) 0.161(2) 0.048 Uiso 1 1 d . U . . .
H26A H 0.465(5) 0.123(3) 0.499(2) 0.048 Uiso 1 1 d . U . . .
C11 C 0.9214(3) 0.6318(2) 0.43207(15) 0.0270(5) Uani 1 1 d . . . . .
C12 C 0.8546(3) 0.4932(2) 0.36678(16) 0.0287(6) Uani 1 1 d . . . . .
C13 C 0.6540(3) 0.6204(2) 0.52764(14) 0.0249(5) Uani 1 1 d . . . . .
H13 H 0.740386 0.614032 0.544887 0.030 Uiso 1 1 calc R U . . .
C14 C 0.5541(3) 0.6153(2) 0.57970(15) 0.0282(6) Uani 1 1 d . . . . .
H14 H 0.572549 0.605711 0.631629 0.034 Uiso 1 1 calc R U . . .
C15 C 0.4304(3) 0.6241(2) 0.55521(15) 0.0274(6) Uani 1 1 d . . . . .
H15 H 0.362095 0.620964 0.590262 0.033 Uiso 1 1 calc R U . . .
C16 C 0.4027(3) 0.6379(2) 0.47792(15) 0.0239(5) Uani 1 1 d . . . . .
C17 C 0.5073(3) 0.64365(19) 0.42895(14) 0.0203(5) Uani 1 1 d . . . . .
C18 C 0.4939(3) 0.6587(2) 0.34662(14) 0.0220(5) Uani 1 1 d . . . . .
C19 C 0.0755(3) 0.8928(2) 0.23511(16) 0.0310(6) Uani 1 1 d . . . . .
C20 C 0.0818(3) 0.8846(2) 0.08966(14) 0.0236(5) Uani 1 1 d . . . . .
C21 C 0.1026(3) 1.0495(2) 0.13720(15) 0.0253(5) Uani 1 1 d . . . . .
C22 C 0.3772(3) 0.8810(2) 0.01208(14) 0.0272(6) Uani 1 1 d . . . . .
H22 H 0.297923 0.882903 -0.011655 0.033 Uiso 1 1 calc R U . . .
C23 C 0.4963(3) 0.8637(2) -0.02886(15) 0.0302(6) Uani 1 1 d . . . . .
H23 H 0.497942 0.852749 -0.079745 0.036 Uiso 1 1 calc R U . . .
C24 C 0.6104(3) 0.8624(2) 0.00424(15) 0.0288(6) Uani 1 1 d . . . . .
H24 H 0.691688 0.850150 -0.023562 0.035 Uiso 1 1 calc R U . . .
C25 C 0.6079(3) 0.8794(2) 0.07961(15) 0.0257(5) Uani 1 1 d . . . . .
C26 C 0.4851(3) 0.89401(19) 0.11801(14) 0.0213(5) Uani 1 1 d . . . . .
C27 C 0.4704(3) 0.90462(19) 0.19904(13) 0.0206(5) Uani 1 1 d . . . . .
C28 C 0.4681(3) 0.1462(3) 0.32528(18) 0.0425(8) Uani 1 1 d . . . . .
C29 C 0.2884(3) 0.1531(2) 0.23179(15) 0.0239(5) Uani 1 1 d . . . . .
C30 C 0.2285(3) 0.3079(3) 0.31665(15) 0.0308(6) Uani 1 1 d . . . . .
C31 C -0.0127(3) 0.1648(2) 0.32121(15) 0.0270(5) Uani 1 1 d . . . . .
H31 H 0.002614 0.175040 0.269099 0.032 Uiso 1 1 calc R U . . .
C32 C -0.1366(3) 0.1590(2) 0.34655(17) 0.0316(6) Uani 1 1 d . . . . .
H32 H -0.204721 0.165079 0.311924 0.038 Uiso 1 1 calc R U . . .
C33 C -0.1593(3) 0.1447(2) 0.42150(18) 0.0313(6) Uani 1 1 d . . . . .
H33 H -0.244163 0.142008 0.438817 0.038 Uiso 1 1 calc R U . . .
C34 C -0.0581(3) 0.1337(2) 0.47324(15) 0.0254(5) Uani 1 1 d . . . . .
C35 C 0.0642(3) 0.14108(19) 0.44347(14) 0.0200(5) Uani 1 1 d . . . . .
C36 C 0.1808(3) 0.1310(2) 0.49025(14) 0.0226(5) Uani 1 1 d . . . . .
N1 N 0.8402(2) 0.38001(16) 0.08918(11) 0.0184(4) Uani 1 1 d . . . . .
N2 N 1.0531(3) 0.3515(2) -0.07691(15) 0.0321(5) Uani 1 1 d . . . . .
N3 N 0.6309(2) 0.63396(17) 0.45463(11) 0.0203(4) Uani 1 1 d . . . . .
N4 N 0.2814(3) 0.6439(2) 0.45410(17) 0.0347(6) Uani 1 1 d . . . . .
N5 N 0.3725(2) 0.89495(16) 0.08384(11) 0.0202(4) Uani 1 1 d . . . . .
N6 N 0.7200(3) 0.8779(3) 0.11323(17) 0.0429(7) Uani 1 1 d . . . . .
N7 N 0.0841(2) 0.15606(17) 0.36876(12) 0.0206(4) Uani 1 1 d . . . . .
N8 N -0.0773(3) 0.1157(2) 0.54736(15) 0.0330(5) Uani 1 1 d . . . . .
O1 O 0.3515(2) 0.3749(2) 0.13205(15) 0.0457(6) Uani 1 1 d . . . . .
O2 O 0.6250(3) 0.4213(2) 0.27548(11) 0.0425(5) Uani 1 1 d . . . . .
O3 O 0.7389(2) 0.13736(18) 0.16477(13) 0.0410(5) Uani 1 1 d . . . . .
O4 O 0.5841(2) 0.54815(16) 0.06783(11) 0.0244(4) Uani 1 1 d . . . . .
O5 O 0.7966(2) 0.36480(15) -0.10113(10) 0.0271(4) Uani 1 1 d . . . . .
O6 O 0.66329(18) 0.36537(15) -0.00309(9) 0.0232(4) Uani 1 1 d . . . . .
O7 O 0.9609(3) 0.6732(2) 0.23859(13) 0.0513(6) Uani 1 1 d . . . . .
O8 O 1.0086(2) 0.6227(2) 0.47169(13) 0.0412(5) Uani 1 1 d . . . . .
O9 O 0.8998(2) 0.40190(18) 0.36536(15) 0.0447(6) Uani 1 1 d . . . . .
O10 O 0.6656(2) 0.81574(15) 0.37058(11) 0.0250(4) Uani 1 1 d . . . . .
O11 O 0.3861(2) 0.66608(17) 0.31767(11) 0.0320(4) Uani 1 1 d . . . . .
O12 O 0.59792(19) 0.66338(15) 0.30892(9) 0.0240(4) Uani 1 1 d . . . . .
O13 O -0.0014(3) 0.8904(2) 0.28149(14) 0.0513(6) Uani 1 1 d . . . . .
O14 O 0.0053(2) 0.87988(17) 0.04753(12) 0.0339(4) Uani 1 1 d . . . . .
O15 O 0.0373(2) 1.13845(16) 0.12350(13) 0.0355(5) Uani 1 1 d . . . . .
O16 O 0.3311(2) 0.72971(15) 0.17596(10) 0.0251(4) Uani 1 1 d . . . . .
O17 O 0.5644(2) 0.91015(16) 0.23463(10) 0.0289(4) Uani 1 1 d . . . . .
O18 O 0.35627(18) 0.90735(14) 0.22875(9) 0.0218(4) Uani 1 1 d . . . . .
O19 O 0.5781(3) 0.1426(3) 0.31761(17) 0.0720(10) Uani 1 1 d . . . . .
O20 O 0.2980(2) 0.15225(16) 0.16824(10) 0.0298(4) Uani 1 1 d . . . . .
O21 O 0.1938(3) 0.39908(19) 0.30335(14) 0.0461(6) Uani 1 1 d . . . . .
O22 O 0.3247(2) -0.01773(16) 0.36359(11) 0.0290(4) Uani 1 1 d . . . . .
O23 O 0.1786(2) 0.11041(18) 0.55928(11) 0.0342(5) Uani 1 1 d . . . . .
O24 O 0.28353(19) 0.14341(16) 0.45545(10) 0.0265(4) Uani 1 1 d . . . . .
O25 O 0.6797(2) 0.63864(17) 0.16379(12) 0.0322(4) Uani 1 1 d . . . . .
O26 O 0.5509(2) 0.10227(19) 0.50601(12) 0.0358(5) Uani 1 1 d . . . . .
H26B H 0.587(6) 0.050(5) 0.479(3) 0.088(18) Uiso 1 1 d . . . . .
Re1 Re 0.63907(2) 0.37854(2) 0.11339(2) 0.01944(3) Uani 1 1 d . . . . .
Re2 Re 0.77676(2) 0.64379(2) 0.36873(2) 0.01925(3) Uani 1 1 d . . . . .
Re3 Re 0.20343(2) 0.89939(2) 0.15772(2) 0.01874(3) Uani 1 1 d . . . . .
Re4 Re 0.28417(2) 0.15572(2) 0.33698(2) 0.02171(3) 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
C1 O1 1.148(4) . ?
C1 Re1 1.919(3) . ?
C2 O2 1.150(4) . ?
C2 Re1 1.901(3) . ?
C3 O3 1.151(4) . ?
C3 Re1 1.905(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(4) . ?
C4 N1 1.335(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.370(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.411(4) . ?
C7 C8 1.406(4) . ?
C7 N2 1.355(4) . ?
C8 C9 1.488(3) . ?
C8 N1 1.358(3) . ?
C9 O5 1.235(3) . ?
C9 O6 1.290(3) . ?
C10 O7 1.148(4) . ?
C10 Re2 1.920(3) . ?
C11 O8 1.154(4) . ?
C11 Re2 1.899(3) . ?
C12 O9 1.151(4) . ?
C12 Re2 1.900(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.400(4) . ?
C13 N3 1.330(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.359(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.415(4) . ?
C16 C17 1.406(4) . ?
C16 N4 1.343(4) . ?
C17 C18 1.482(3) . ?
C17 N3 1.363(3) . ?
C18 O11 1.242(3) . ?
C18 O12 1.286(3) . ?
C19 O13 1.149(4) . ?
C19 Re3 1.922(3) . ?
C20 O14 1.159(3) . ?
C20 Re3 1.898(3) . ?
C21 O15 1.146(3) . ?
C21 Re3 1.908(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.395(4) . ?
C22 N5 1.333(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.366(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.410(4) . ?
C25 C26 1.409(4) . ?
C25 N6 1.349(4) . ?
C26 C27 1.488(3) . ?
C26 N5 1.362(3) . ?
C27 O17 1.238(3) . ?
C27 O18 1.291(3) . ?
C28 O19 1.150(4) . ?
C28 Re4 1.909(3) . ?
C29 O20 1.151(3) . ?
C29 Re4 1.906(3) . ?
C30 O21 1.142(4) . ?
C30 Re4 1.906(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.395(4) . ?
C31 N7 1.330(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.367(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.408(4) . ?
C34 C35 1.412(4) . ?
C34 N8 1.350(4) . ?
C35 C36 1.482(3) . ?
C35 N7 1.358(3) . ?
C36 O23 1.243(3) . ?
C36 O24 1.285(3) . ?
N1 Re1 2.162(2) . ?
N2 H2A 0.88(4) . ?
N2 H2B 0.82(4) . ?
N3 Re2 2.169(2) . ?
N4 H4C 0.83(4) . ?
N4 H4D 0.91(4) . ?
N5 Re3 2.175(2) . ?
N6 H6A 0.85(4) . ?
N6 H6B 0.81(4) . ?
N7 Re4 2.169(2) . ?
N8 H8A 0.87(4) . ?
N8 H8B 0.80(4) . ?
O4 H4A 0.76(4) . ?
O4 H4B 0.77(5) . ?
O4 Re1 2.195(2) . ?
O6 Re1 2.1353(17) . ?
O10 H10A 0.79(5) . ?
O10 H10B 0.78(5) . ?
O10 Re2 2.1916(19) . ?
O12 Re2 2.1364(17) . ?
O16 H16A 0.87(4) . ?
O16 H16B 0.91(4) . ?
O16 Re3 2.1836(19) . ?
O18 Re3 2.1501(17) . ?
O22 H22A 0.82(5) . ?
O22 H22B 0.80(4) . ?
O22 Re4 2.207(2) . ?
O24 Re4 2.1273(18) . ?
O25 H25A 0.89(4) . ?
O25 H25B 0.73(5) . ?
O26 H26A 0.86(5) . ?
O26 H26B 0.87(6) . ?

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
O1 C1 Re1 177.0(3) . . ?
O2 C2 Re1 178.4(3) . . ?
O3 C3 Re1 179.6(3) . . ?
C5 C4 H4 119.4 . . ?
N1 C4 H4 119.4 . . ?
N1 C4 C5 121.2(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.5(2) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.4(2) . . ?
C7 C6 H6 119.8 . . ?
C8 C7 C6 117.0(2) . . ?
N2 C7 C6 120.7(3) . . ?
N2 C7 C8 122.3(3) . . ?
C7 C8 C9 123.6(2) . . ?
N1 C8 C7 121.4(2) . . ?
N1 C8 C9 115.0(2) . . ?
O5 C9 C8 120.8(2) . . ?
O5 C9 O6 122.9(2) . . ?
O6 C9 C8 116.4(2) . . ?
O7 C10 Re2 178.2(3) . . ?
O8 C11 Re2 178.4(3) . . ?
O9 C12 Re2 178.9(3) . . ?
C14 C13 H13 119.2 . . ?
N3 C13 H13 119.2 . . ?
N3 C13 C14 121.6(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.5(3) . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 117.0(2) . . ?
N4 C16 C15 120.2(3) . . ?
N4 C16 C17 122.8(3) . . ?
C16 C17 C18 123.5(2) . . ?
N3 C17 C16 121.6(2) . . ?
N3 C17 C18 114.9(2) . . ?
O11 C18 C17 119.8(2) . . ?
O11 C18 O12 123.6(2) . . ?
O12 C18 C17 116.6(2) . . ?
O13 C19 Re3 178.9(3) . . ?
O14 C20 Re3 177.4(2) . . ?
O15 C21 Re3 176.8(2) . . ?
C23 C22 H22 119.3 . . ?
N5 C22 H22 119.3 . . ?
N5 C22 C23 121.3(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.1(3) . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 116.9(3) . . ?
N6 C25 C24 120.8(3) . . ?
N6 C25 C26 122.2(3) . . ?
C25 C26 C27 122.8(2) . . ?
N5 C26 C25 122.0(2) . . ?
N5 C26 C27 115.2(2) . . ?
O17 C27 C26 120.4(2) . . ?
O17 C27 O18 123.2(2) . . ?
O18 C27 C26 116.4(2) . . ?
O19 C28 Re4 178.6(4) . . ?
O20 C29 Re4 176.1(2) . . ?
O21 C30 Re4 178.7(3) . . ?
C32 C31 H31 119.4 . . ?
N7 C31 H31 119.4 . . ?
N7 C31 C32 121.1(3) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 C31 119.6(3) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.6(3) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C35 116.5(2) . . ?
N8 C34 C33 121.2(3) . . ?
N8 C34 C35 122.2(3) . . ?
C34 C35 C36 123.3(2) . . ?
N7 C35 C34 121.8(2) . . ?
N7 C35 C36 114.9(2) . . ?
O23 C36 C35 121.2(2) . . ?
O23 C36 O24 122.4(2) . . ?
O24 C36 C35 116.3(2) . . ?
C4 N1 C8 120.5(2) . . ?
C4 N1 Re1 124.59(17) . . ?
C8 N1 Re1 114.94(16) . . ?
C7 N2 H2A 118(3) . . ?
C7 N2 H2B 116(3) . . ?
H2A N2 H2B 121(4) . . ?
C13 N3 C17 119.9(2) . . ?
C13 N3 Re2 125.06(18) . . ?
C17 N3 Re2 115.01(16) . . ?
H4C N4 H4D 120(4) . . ?
C16 N4 H4C 123(3) . . ?
C16 N4 H4D 117(3) . . ?
C22 N5 C26 119.7(2) . . ?
C22 N5 Re3 124.82(19) . . ?
C26 N5 Re3 114.97(16) . . ?
H6A N6 H6B 119(4) . . ?
C25 N6 H6A 118(3) . . ?
C25 N6 H6B 121(3) . . ?
C31 N7 C35 120.3(2) . . ?
C31 N7 Re4 124.85(18) . . ?
C35 N7 Re4 114.75(16) . . ?
H8A N8 H8B 120(4) . . ?
C34 N8 H8A 121(3) . . ?
C34 N8 H8B 119(3) . . ?
H4A O4 H4B 111(4) . . ?
Re1 O4 H4A 111(3) . . ?
Re1 O4 H4B 115(3) . . ?
C9 O6 Re1 117.76(15) . . ?
H10A O10 H10B 108(4) . . ?
Re2 O10 H10A 112(3) . . ?
Re2 O10 H10B 115(3) . . ?
C18 O12 Re2 118.14(15) . . ?
H16A O16 H16B 103(4) . . ?
Re3 O16 H16A 110(3) . . ?
Re3 O16 H16B 112(3) . . ?
C27 O18 Re3 117.94(15) . . ?
H22A O22 H22B 109(4) . . ?
Re4 O22 H22A 118(3) . . ?
Re4 O22 H22B 112(3) . . ?
C36 O24 Re4 118.09(15) . . ?
H25A O25 H25B 94(4) . . ?
H26A O26 H26B 106(4) . . ?
C1 Re1 N1 174.05(10) . . ?
C1 Re1 O4 96.71(10) . . ?
C1 Re1 O6 98.41(10) . . ?
C2 Re1 C1 87.42(12) . . ?
C2 Re1 C3 89.50(12) . . ?
C2 Re1 N1 98.30(10) . . ?
C2 Re1 O4 94.62(10) . . ?
C2 Re1 O6 172.17(10) . . ?
C3 Re1 C1 87.83(12) . . ?
C3 Re1 N1 93.83(10) . . ?
C3 Re1 O4 173.98(10) . . ?
C3 Re1 O6 95.90(9) . . ?
N1 Re1 O4 81.26(7) . . ?
O6 Re1 N1 75.74(7) . . ?
O6 Re1 O4 79.57(7) . . ?
C10 Re2 N3 173.98(11) . . ?
C10 Re2 O10 94.80(11) . . ?
C10 Re2 O12 99.58(10) . . ?
C11 Re2 C10 86.88(12) . . ?
C11 Re2 C12 88.33(12) . . ?
C11 Re2 N3 98.00(10) . . ?
C11 Re2 O10 96.73(10) . . ?
C11 Re2 O12 172.89(10) . . ?
C12 Re2 C10 89.02(13) . . ?
C12 Re2 N3 94.60(10) . . ?
C12 Re2 O10 173.80(10) . . ?
C12 Re2 O12 94.70(10) . . ?
N3 Re2 O10 81.19(8) . . ?
O12 Re2 N3 75.37(7) . . ?
O12 Re2 O10 79.87(7) . . ?
C19 Re3 N5 170.93(10) . . ?
C19 Re3 O16 96.30(10) . . ?
C19 Re3 O18 96.66(10) . . ?
C20 Re3 C19 87.66(12) . . ?
C20 Re3 C21 84.97(11) . . ?
C20 Re3 N5 100.09(10) . . ?
C20 Re3 O16 96.19(9) . . ?
C20 Re3 O18 174.69(9) . . ?
C21 Re3 C19 87.95(12) . . ?
C21 Re3 N5 97.35(10) . . ?
C21 Re3 O16 175.63(10) . . ?
C21 Re3 O18 98.23(9) . . ?
N5 Re3 O16 78.31(8) . . ?
O18 Re3 N5 75.36(7) . . ?
O18 Re3 O16 80.31(7) . . ?
C28 Re4 N7 170.79(11) . . ?
C28 Re4 O22 97.30(13) . . ?
C28 Re4 O24 95.85(11) . . ?
C29 Re4 C28 84.62(12) . . ?
C29 Re4 N7 103.87(9) . . ?
C29 Re4 O22 94.07(9) . . ?
C29 Re4 O24 174.84(10) . . ?
C30 Re4 C28 89.06(15) . . ?
C30 Re4 C29 87.34(11) . . ?
C30 Re4 N7 94.82(11) . . ?
C30 Re4 O22 173.58(10) . . ?
C30 Re4 O24 97.80(10) . . ?
N7 Re4 O22 78.76(8) . . ?
O24 Re4 N7 75.37(7) . . ?
O24 Re4 O22 80.77(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
C5 H5 O1 0.95 2.49 3.126(3) 123.9 1_655 yes
C6 H6 O1 0.95 2.56 3.161(3) 121.2 1_655 yes
N2 H2A O5 0.88(4) 2.04(4) 2.707(3) 132(4) . yes
N2 H2A O7 0.88(4) 2.41(4) 3.004(4) 126(3) 2_765 yes
N2 H2B O25 0.82(4) 2.44(4) 3.213(3) 157(4) 2_765 yes
N4 H4C O8 0.83(4) 2.36(4) 3.004(3) 135(4) 1_455 yes
N4 H4D O11 0.91(4) 1.99(4) 2.686(4) 133(4) . yes
N6 H6A O17 0.85(4) 2.04(4) 2.674(4) 131(4) . yes
N6 H6B O14 0.81(4) 2.42(4) 3.206(4) 164(4) 1_655 yes
N8 H8A O13 0.87(4) 2.54(4) 3.224(4) 136(4) 2_566 yes
N8 H8A O23 0.87(4) 2.07(4) 2.702(4) 129(4) . yes
O4 H4A O25 0.76(4) 1.93(5) 2.672(3) 165(4) . yes
O4 H4B O6 0.77(5) 1.93(5) 2.699(3) 174(4) 2_665 yes
O10 H10A O17 0.79(5) 1.90(5) 2.687(3) 170(4) . yes
O10 H10B O23 0.78(5) 1.88(5) 2.651(3) 168(4) 2_666 yes
O16 H16A O5 0.87(4) 1.84(4) 2.674(3) 162(4) 2_665 yes
O16 H16B O11 0.91(4) 1.70(4) 2.612(3) 173(4) . yes
O22 H22A O26 0.82(5) 1.87(5) 2.657(3) 162(4) 2_656 yes
O22 H22B O18 0.80(4) 1.95(5) 2.726(3) 165(4) 1_545 yes
O25 H25A O12 0.89(4) 1.89(5) 2.754(3) 164(4) . yes
O26 H26A O24 0.86(5) 2.02(5) 2.848(3) 161(4) . yes
C15 H15 O2 0.95 2.42 3.115(3) 130.1 2_666 yes
C23 H23 O20 0.95 2.62 3.238(3) 123.1 2_665 yes
C24 H24 O20 0.95 2.62 3.238(3) 123.1 2_665 yes
C32 H32 O19 0.95 2.42 3.178(4) 136.4 1_455 yes

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
C4 C5 C6 C7 0.7(4) . . . . ?
C5 C4 N1 C8 -0.2(4) . . . . ?
C5 C4 N1 Re1 178.37(18) . . . . ?
C5 C6 C7 C8 0.5(4) . . . . ?
C5 C6 C7 N2 -178.7(3) . . . . ?
C6 C7 C8 C9 177.6(2) . . . . ?
C6 C7 C8 N1 -1.6(4) . . . . ?
C7 C8 C9 O5 -3.9(4) . . . . ?
C7 C8 C9 O6 175.8(2) . . . . ?
C7 C8 N1 C4 1.5(3) . . . . ?
C7 C8 N1 Re1 -177.19(18) . . . . ?
C8 C9 O6 Re1 3.9(3) . . . . ?
C9 C8 N1 C4 -177.8(2) . . . . ?
C9 C8 N1 Re1 3.5(3) . . . . ?
C13 C14 C15 C16 0.2(4) . . . . ?
C14 C13 N3 C17 0.3(4) . . . . ?
C14 C13 N3 Re2 179.7(2) . . . . ?
C14 C15 C16 C17 -1.0(4) . . . . ?
C14 C15 C16 N4 178.3(3) . . . . ?
C15 C16 C17 C18 -179.5(2) . . . . ?
C15 C16 C17 N3 1.4(4) . . . . ?
C16 C17 C18 O11 -0.6(4) . . . . ?
C16 C17 C18 O12 179.4(2) . . . . ?
C16 C17 N3 C13 -1.1(4) . . . . ?
C16 C17 N3 Re2 179.40(18) . . . . ?
C17 C18 O12 Re2 2.0(3) . . . . ?
C18 C17 N3 C13 179.8(2) . . . . ?
C18 C17 N3 Re2 0.3(3) . . . . ?
C22 C23 C24 C25 -0.4(4) . . . . ?
C23 C22 N5 C26 1.0(4) . . . . ?
C23 C22 N5 Re3 -170.6(2) . . . . ?
C23 C24 C25 C26 1.8(4) . . . . ?
C23 C24 C25 N6 179.7(3) . . . . ?
C24 C25 C26 C27 175.4(2) . . . . ?
C24 C25 C26 N5 -1.8(4) . . . . ?
C25 C26 C27 O17 6.3(4) . . . . ?
C25 C26 C27 O18 -173.6(2) . . . . ?
C25 C26 N5 C22 0.4(4) . . . . ?
C25 C26 N5 Re3 172.90(18) . . . . ?
C26 C27 O18 Re3 -1.2(3) . . . . ?
C27 C26 N5 C22 -176.9(2) . . . . ?
C27 C26 N5 Re3 -4.5(3) . . . . ?
C31 C32 C33 C34 -1.1(4) . . . . ?
C32 C31 N7 C35 0.2(4) . . . . ?
C32 C31 N7 Re4 176.9(2) . . . . ?
C32 C33 C34 C35 1.5(4) . . . . ?
C32 C33 C34 N8 -177.6(3) . . . . ?
C33 C34 C35 C36 -179.8(2) . . . . ?
C33 C34 C35 N7 -1.1(4) . . . . ?
C34 C35 C36 O23 3.3(4) . . . . ?
C34 C35 C36 O24 -177.5(2) . . . . ?
C34 C35 N7 C31 0.3(4) . . . . ?
C34 C35 N7 Re4 -176.73(18) . . . . ?
C35 C36 O24 Re4 -7.9(3) . . . . ?
C36 C35 N7 C31 179.1(2) . . . . ?
C36 C35 N7 Re4 2.1(3) . . . . ?
N1 C4 C5 C6 -0.9(4) . . . . ?
N1 C8 C9 O5 175.4(2) . . . . ?
N1 C8 C9 O6 -4.9(3) . . . . ?
N2 C7 C8 C9 -3.2(4) . . . . ?
N2 C7 C8 N1 177.5(2) . . . . ?
N3 C13 C14 C15 0.2(4) . . . . ?
N3 C17 C18 O11 178.5(2) . . . . ?
N3 C17 C18 O12 -1.5(3) . . . . ?
N4 C16 C17 C18 1.1(4) . . . . ?
N4 C16 C17 N3 -177.9(2) . . . . ?
N5 C22 C23 C24 -1.0(4) . . . . ?
N5 C26 C27 O17 -176.3(2) . . . . ?
N5 C26 C27 O18 3.8(3) . . . . ?
N6 C25 C26 C27 -2.5(4) . . . . ?
N6 C25 C26 N5 -179.7(3) . . . . ?
N7 C31 C32 C33 0.3(4) . . . . ?
N7 C35 C36 O23 -175.5(2) . . . . ?
N7 C35 C36 O24 3.7(3) . . . . ?
N8 C34 C35 C36 -0.7(4) . . . . ?
N8 C34 C35 N7 178.0(2) . . . . ?
O5 C9 O6 Re1 -176.45(18) . . . . ?
O11 C18 O12 Re2 -178.0(2) . . . . ?
O17 C27 O18 Re3 178.99(19) . . . . ?
O23 C36 O24 Re4 171.3(2) . . . . ?


####################################################################### 
# 
# 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_39
_database_code_depnum_ccdc_archive 'CCDC 2205525'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O7 Re, H2 O'
_chemical_formula_sum            'C10 H10 N O8 Re'
_chemical_formula_weight         458.39
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.88210(10)
_cell_length_b                   11.1360(2)
_cell_length_c                   26.3990(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.4570(10)
_cell_angle_gamma                90
_cell_volume                     2606.40(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    11907
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3530
_cell_measurement_theta_min      3.3060
_shelx_estimated_absorpt_T_max   0.355
_shelx_estimated_absorpt_T_min   0.118
_exptl_absorpt_coefficient_mu    18.634
_exptl_absorpt_correction_T_max  0.426
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.0407
0 1 1 0.0347
0 -5 3 0.0469
0 5 -3 0.0229
1 0 0 0.0870
-1 0 0 0.1030
0 1 -5 0.0704
0 -1 5 0.0704

_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07

_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13294
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         3.354
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -7.00   0.80    1.00    --  -42.49 125.00 -60.00  100
  2  ω   -115.00 -20.60   0.80    1.00    --  -42.49 -37.00 150.00  118
  3  ω     20.00 114.40   0.80    1.00    --   42.49  37.00-120.00  118
  4  ω     27.00  97.40   0.80    1.00    --   42.49-125.00-180.00   88
  5  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00-120.00   95
  6  ω    103.00 177.40   0.80    2.00    --  111.00  77.00 -60.00   93
  7  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00-180.00   95
  8  ω     37.00 141.00   0.80    2.00    --  111.00 -77.00-180.00  130
  9  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00 -30.00   95
 10  ω    103.00 177.40   0.80    2.00    --  111.00  77.00-150.00   93
 11  ω     40.00 134.40   0.80    2.00    --  111.00 -45.00 -30.00  118
 12  ω    104.00 177.60   0.80    2.00    --  111.00 111.00 -60.00   92
 13  ω    103.00 177.40   0.80    2.00    --  111.00  77.00 -30.00   93
 14  ω     36.00 134.40   0.80    2.00    --  111.00 -30.00-180.00  123
 15  ω   -113.00 -17.00   0.80    1.00    --  -42.49 -57.00  60.00  120
 16  ω   -113.00 -17.00   0.80    1.00    --  -42.49 -57.00   0.00  120
 17  ω    -30.00  64.40   0.80    1.00    --   42.49 -37.00-150.00  118
 18  ω     16.00 112.00   0.80    1.00    --   42.49  57.00 -30.00  120
 19  ω     87.00 177.40   0.80    2.00    --  111.00  30.00  60.00  113
 20  ω     83.00 136.60   0.80    2.00    --  111.00  61.00 -90.00   67
 21  ω     87.00 177.40   0.80    2.00    --  111.00  45.00 150.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1284043000
_diffrn_orient_matrix_UB_12      0.0882042000
_diffrn_orient_matrix_UB_13      0.0102333000
_diffrn_orient_matrix_UB_21      0.1170045000
_diffrn_orient_matrix_UB_22      0.0987577000
_diffrn_orient_matrix_UB_23      0.0136007000
_diffrn_orient_matrix_UB_31      -0.0061441000
_diffrn_orient_matrix_UB_32      0.0399786000
_diffrn_orient_matrix_UB_33      -0.0559221000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2640
_reflns_number_total             2652

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.000191(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0164
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+6.5021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0420
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O8-H8A \\sim O8-H8C \\sim O8-H8B
 with sigma of 0.005
3. Others
 Fixed Sof: H8B(0.5) H8A(0.5)
4.a Free rotating group:
 O8(H8B,H8C)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.37362(2) 0.18385(2) 0.62683(2) 0.01962(6) Uani 1 1 d . . . . .
O1 O 0.3862(3) -0.0905(2) 0.62271(9) 0.0425(6) Uani 1 1 d . . . . .
O2 O 0.6410(3) 0.1719(2) 0.70519(9) 0.0408(6) Uani 1 1 d . . . . .
O3 O 0.1594(3) 0.1588(2) 0.71244(9) 0.0422(5) Uani 1 1 d . . . . .
O4 O 0.5181(2) 0.20872(19) 0.56353(8) 0.0252(4) Uani 1 1 d . . . . .
H4A H 0.553(5) 0.145(4) 0.5538(16) 0.047(12) Uiso 1 1 d . . . . .
H4B H 0.487(5) 0.241(4) 0.5386(16) 0.048(12) Uiso 1 1 d . . . . .
O5 O 0.5150(2) 0.41957(18) 0.68280(7) 0.0295(4) Uani 1 1 d . . . . .
O6 O 0.0758(2) 0.33911(18) 0.51616(7) 0.0251(4) Uani 1 1 d . . . . .
O7 O 0.2006(2) 0.20930(17) 0.56749(7) 0.0228(4) Uani 1 1 d . . . . .
O8 O 0.6288(3) 0.0071(2) 0.52839(9) 0.0354(5) Uani 1 1 d DG . . . .
H8B H 0.709479 0.022754 0.512452 0.053 Uiso 0.5 1 d DG U P A -1
H8C H 0.644010 -0.064695 0.540650 0.053 Uiso 1 1 d DG U . . .
N1 N 0.3475(2) 0.3801(2) 0.61844(8) 0.0186(4) Uani 1 1 d . . . . .
C1 C 0.3818(3) 0.0129(3) 0.62425(10) 0.0306(6) Uani 1 1 d . . . . .
C2 C 0.5413(4) 0.1766(2) 0.67596(12) 0.0294(6) Uani 1 1 d . . . . .
C3 C 0.2410(4) 0.1690(3) 0.68036(11) 0.0288(6) Uani 1 1 d . . . . .
C4 C 0.4196(3) 0.4647(2) 0.64646(9) 0.0209(5) Uani 1 1 d . . . . .
C5 C 0.3949(3) 0.5874(3) 0.63767(11) 0.0272(6) Uani 1 1 d . . . . .
H5 H 0.447152 0.646077 0.658118 0.033 Uiso 1 1 calc R U . . .
C6 C 0.2943(3) 0.6211(2) 0.59914(12) 0.0300(6) Uani 1 1 d . . . . .
H6 H 0.276610 0.703808 0.592373 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2173(3) 0.5337(2) 0.56961(10) 0.0256(5) Uani 1 1 d . . . . .
H7 H 0.146691 0.555738 0.542752 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2466(3) 0.4159(2) 0.58057(9) 0.0204(5) Uani 1 1 d . . . . .
C9 C 0.1665(3) 0.3157(2) 0.55189(10) 0.0202(5) Uani 1 1 d . . . . .
C10 C 0.5907(3) 0.5000(3) 0.71829(11) 0.0336(6) Uani 1 1 d . . . . .
H10A H 0.654962 0.554798 0.700132 0.050 Uiso 1 1 calc R U . . .
H10B H 0.652998 0.453770 0.743200 0.050 Uiso 1 1 calc R U . . .
H10C H 0.515853 0.546556 0.735783 0.050 Uiso 1 1 calc R U . . .
H8A H 0.562(6) -0.007(8) 0.504(2) 0.050 Uiso 0.5 1 d D U P B -2


_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 O4 2.185(2) . ?
Re1 O7 2.1459(18) . ?
Re1 N1 2.208(2) . ?
Re1 C1 1.906(3) . ?
Re1 C2 1.916(3) . ?
Re1 C3 1.900(3) . ?
O1 C1 1.153(4) . ?
O2 C2 1.141(4) . ?
O3 C3 1.153(4) . ?
O4 H4A 0.82(5) . ?
O4 H4B 0.79(4) . ?
O5 C4 1.339(3) . ?
O5 C10 1.434(3) . ?
O6 C9 1.231(3) . ?
O7 C9 1.284(3) . ?
O8 H8B 0.8699 . ?
O8 H8C 0.8703 . ?
O8 H8A 0.871(5) . ?
N1 C4 1.337(3) . ?
N1 C8 1.361(3) . ?
C4 C5 1.402(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.365(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.399(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.365(4) . ?
C8 C9 1.504(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
O4 Re1 N1 82.00(8) . . ?
O7 Re1 O4 81.53(8) . . ?
O7 Re1 N1 74.31(8) . . ?
C1 Re1 O4 94.23(10) . . ?
C1 Re1 O7 97.65(9) . . ?
C1 Re1 N1 171.51(10) . . ?
C1 Re1 C2 87.26(12) . . ?
C2 Re1 O4 93.14(11) . . ?
C2 Re1 O7 172.97(10) . . ?
C2 Re1 N1 100.50(10) . . ?
C3 Re1 O4 176.86(10) . . ?
C3 Re1 O7 96.07(11) . . ?
C3 Re1 N1 95.42(10) . . ?
C3 Re1 C1 88.08(12) . . ?
C3 Re1 C2 89.09(13) . . ?
Re1 O4 H4A 112(3) . . ?
Re1 O4 H4B 120(3) . . ?
H4A O4 H4B 105(4) . . ?
C4 O5 C10 119.0(2) . . ?
C9 O7 Re1 120.03(17) . . ?
H8B O8 H8C 104.5 . . ?
H8C O8 H8A 101.7 . . ?
C4 N1 Re1 126.71(17) . . ?
C4 N1 C8 118.2(2) . . ?
C8 N1 Re1 115.11(17) . . ?
O1 C1 Re1 179.7(3) . . ?
O2 C2 Re1 179.8(3) . . ?
O3 C3 Re1 179.0(3) . . ?
O5 C4 C5 124.8(2) . . ?
N1 C4 O5 113.2(2) . . ?
N1 C4 C5 122.0(2) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.7(3) . . ?
C6 C5 H5 120.7 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.1(3) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 121.0 . . ?
C8 C7 C6 118.0(2) . . ?
C8 C7 H7 121.0 . . ?
N1 C8 C7 123.1(2) . . ?
N1 C8 C9 115.0(2) . . ?
C7 C8 C9 121.9(2) . . ?
O6 C9 O7 124.9(2) . . ?
O6 C9 C8 119.8(2) . . ?
O7 C9 C8 115.3(2) . . ?
O5 C10 H10A 109.5 . . ?
O5 C10 H10B 109.5 . . ?
O5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
O4 H4A O8 0.82(5) 1.82(5) 2.642(3) 176(4) . yes
O4 H4B O6 0.79(4) 1.87(5) 2.649(3) 172(5) 2_556 yes
C6 H6 O4 0.95 2.57 3.197(3) 124.0 6_565 yes

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
Re1 O7 C9 O6 175.4(2) . . . . ?
Re1 O7 C9 C8 -4.5(3) . . . . ?
Re1 N1 C4 O5 -0.4(3) . . . . ?
Re1 N1 C4 C5 179.66(18) . . . . ?
Re1 N1 C8 C7 -179.3(2) . . . . ?
Re1 N1 C8 C9 1.8(3) . . . . ?
O5 C4 C5 C6 179.9(3) . . . . ?
N1 C4 C5 C6 -0.2(4) . . . . ?
N1 C8 C9 O6 -178.3(2) . . . . ?
N1 C8 C9 O7 1.6(3) . . . . ?
C4 N1 C8 C7 0.8(4) . . . . ?
C4 N1 C8 C9 -178.1(2) . . . . ?
C4 C5 C6 C7 0.5(4) . . . . ?
C5 C6 C7 C8 -0.2(4) . . . . ?
C6 C7 C8 N1 -0.4(4) . . . . ?
C6 C7 C8 C9 178.4(2) . . . . ?
C7 C8 C9 O6 2.8(4) . . . . ?
C7 C8 C9 O7 -177.3(2) . . . . ?
C8 N1 C4 O5 179.5(2) . . . . ?
C8 N1 C4 C5 -0.4(4) . . . . ?
C10 O5 C4 N1 -175.0(2) . . . . ?
C10 O5 C4 C5 4.9(4) . . . . ?


####################################################################### 
# 
# 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_34
_database_code_depnum_ccdc_archive 'CCDC 2205519'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H5 F3 N O6 Re'
_chemical_formula_sum            'C10 H5 F3 N O6 Re'
_chemical_formula_weight         478.35
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   12.92600(10)
_cell_length_b                   6.81770(10)
_cell_length_c                   15.2153(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.2060(10)
_cell_angle_gamma                90
_cell_volume                     1241.41(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10876
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.2270
_cell_measurement_theta_min      3.1040
_shelx_estimated_absorpt_T_max   0.504
_shelx_estimated_absorpt_T_min   0.049
_exptl_absorpt_coefficient_mu    19.846
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.087
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0275
0 0 -1 0.0105
-5 0 3 0.0529
5 0 -3 0.0529
1 4 -1 0.1761
-4 -4 -1 0.1438
6 -1 3 0.0799

_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04

_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.312
_diffrn_reflns_theta_min         3.838
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -16.00   1.00    1.00    --  -42.61 -57.00  30.00   97
  2  ω      6.00  83.00   1.00    1.00    --   42.61 -99.00  90.00   77
  3  ω    -21.00  74.00   1.00    1.00    --   42.61 -77.00-120.00   95
  4  ω     11.00  42.00   1.00    1.00    --   42.61  77.00  -1.50   31
  5  ω     30.00 107.00   1.00    1.00    --  111.00 -94.00 -90.00   77
  6  ω     82.00 178.00   1.00    1.00    --  111.00  68.00 143.32   96
  7  ω     37.00 142.00   1.00    1.00    --  111.00 -77.00   0.00  105
  8  ω    103.00 178.00   1.00    1.00    --  111.00  77.00   0.00   75
  9  ω     39.00 111.00   1.00    1.00    --  111.00-121.00-115.00   72
 10  ω     36.00 109.00   1.00    1.00    --  111.00-111.00 120.00   73
 11  ω     36.00 109.00   1.00    1.00    --  111.00-111.00   0.00   73
 12  ω     36.00 109.00   1.00    1.00    --  111.00-111.00 -90.00   73
 13  ω     40.00 135.00   1.00    1.00    --  111.00 -45.00 -30.00   95
 14  ω     83.00 178.00   1.00    1.00    --  111.00  61.00 120.00   95
 15  ω   -116.00 -20.00   1.00    1.00    --  -42.61 -37.00 -60.00   96
 16  ω   -113.00 -16.00   1.00    1.00    --  -42.61 -57.00-150.00   97
 17  ω     10.00  42.00   1.00    1.00    --   42.61  81.00 141.98   32
 18  ω     87.00 178.00   1.00    1.00    --  111.00  30.00-120.00   91
 19  ω     82.00 178.00   1.00    1.00    --  111.00  69.00  62.78   96
 20  ω     81.00 178.00   1.00    1.00    --  111.00  71.00 -23.81   97
 21  ω     83.00 116.00   1.00    1.00    --  111.00  61.00-180.00   33
 22  ω     87.00 178.00   1.00    1.00    --  111.00  45.00 -60.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0326872000
_diffrn_orient_matrix_UB_12      0.0619348000
_diffrn_orient_matrix_UB_13      0.0834948000
_diffrn_orient_matrix_UB_21      -0.0238467000
_diffrn_orient_matrix_UB_22      -0.2158298000
_diffrn_orient_matrix_UB_23      0.0157717000
_diffrn_orient_matrix_UB_31      0.1221215000
_diffrn_orient_matrix_UB_32      -0.0253937000
_diffrn_orient_matrix_UB_33      0.0688932000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2523
_reflns_number_total             2583

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00084(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2583
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0264P)²+0.8546P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0440
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.34465(2) 0.38354(2) 0.56029(2) 0.02004(7) Uani 1 1 d . . . . .
F1 F 0.07753(15) 0.2718(3) 0.53755(13) 0.0399(4) Uani 1 1 d . . . . .
F2 F 0.10550(17) 0.0839(3) 0.43477(13) 0.0395(4) Uani 1 1 d . . . . .
F3 F -0.05610(16) 0.2109(4) 0.40516(17) 0.0583(6) Uani 1 1 d . . . . .
O1 O 0.57448(17) 0.3324(3) 0.71786(15) 0.0329(4) Uani 1 1 d . . . . .
O2 O 0.28728(17) -0.0273(3) 0.60977(14) 0.0310(4) Uani 1 1 d . . . . .
O3 O 0.27249(18) 0.5511(4) 0.71455(15) 0.0374(5) Uani 1 1 d . . . . .
O4 O 0.38650(16) 0.2814(3) 0.44096(13) 0.0232(4) Uani 1 1 d . . . . .
H4A H 0.370(3) 0.163(6) 0.433(3) 0.039(10) Uiso 1 1 d . . . . .
H4B H 0.460(4) 0.302(7) 0.454(3) 0.051(11) Uiso 1 1 d . . . . .
O5 O 0.3480(2) 0.8972(3) 0.41353(17) 0.0329(5) Uani 1 1 d . . . . .
O6 O 0.39584(16) 0.6508(3) 0.51711(14) 0.0244(4) Uani 1 1 d . . . . .
N1 N 0.19066(18) 0.4904(3) 0.43877(15) 0.0219(4) Uani 1 1 d . . . . .
C1 C 0.4879(2) 0.3443(4) 0.65738(19) 0.0255(5) Uani 1 1 d . . . . .
C2 C 0.3057(2) 0.1273(4) 0.59024(19) 0.0244(5) Uani 1 1 d . . . . .
C3 C 0.2988(2) 0.4883(4) 0.65569(19) 0.0274(5) Uani 1 1 d . . . . .
C4 C 0.0852(2) 0.4219(4) 0.3999(2) 0.0253(5) Uani 1 1 d . . . . .
C5 C 0.0041(2) 0.5029(4) 0.3200(2) 0.0293(6) Uani 1 1 d . . . . .
H5 H -0.069820 0.452061 0.296344 0.035 Uiso 1 1 calc R U . . .
C6 C 0.0321(3) 0.6585(5) 0.2752(2) 0.0356(6) Uani 1 1 d . . . . .
H6 H -0.020856 0.712290 0.218403 0.043 Uiso 1 1 calc R U . . .
C7 C 0.1390(3) 0.7340(4) 0.3152(2) 0.0328(6) Uani 1 1 d . . . . .
H7 H 0.160484 0.842707 0.286849 0.039 Uiso 1 1 calc R U . . .
C8 C 0.2144(2) 0.6492(4) 0.3969(2) 0.0245(5) Uani 1 1 d . . . . .
C9 C 0.3272(2) 0.7435(4) 0.44445(19) 0.0248(5) Uani 1 1 d . . . . .
C10 C 0.0534(2) 0.2468(5) 0.4450(2) 0.0332(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 O4 2.1948(18) . ?
Re1 O6 2.1257(18) . ?
Re1 N1 2.265(2) . ?
Re1 C1 1.901(3) . ?
Re1 C2 1.920(3) . ?
Re1 C3 1.902(3) . ?
F1 C10 1.334(3) . ?
F2 C10 1.338(4) . ?
F3 C10 1.335(3) . ?
O1 C1 1.152(4) . ?
O2 C2 1.144(3) . ?
O3 C3 1.154(3) . ?
O4 H4A 0.83(4) . ?
O4 H4B 0.91(4) . ?
O5 C9 1.219(3) . ?
O6 C9 1.291(3) . ?
N1 C4 1.348(3) . ?
N1 C8 1.349(3) . ?
C4 C5 1.385(4) . ?
C4 C10 1.509(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(4) . ?
C8 C9 1.506(4) . ?

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
O4 Re1 N1 80.92(7) . . ?
O6 Re1 O4 79.25(7) . . ?
O6 Re1 N1 75.64(8) . . ?
C1 Re1 O4 97.24(10) . . ?
C1 Re1 O6 92.03(10) . . ?
C1 Re1 N1 167.67(10) . . ?
C1 Re1 C2 87.31(12) . . ?
C1 Re1 C3 87.27(12) . . ?
C2 Re1 O4 94.37(10) . . ?
C2 Re1 O6 173.46(10) . . ?
C2 Re1 N1 104.96(10) . . ?
C3 Re1 O4 174.70(10) . . ?
C3 Re1 O6 97.87(10) . . ?
C3 Re1 N1 94.08(10) . . ?
C3 Re1 C2 88.59(12) . . ?
Re1 O4 H4A 108(3) . . ?
Re1 O4 H4B 110(3) . . ?
H4A O4 H4B 111(4) . . ?
C9 O6 Re1 119.42(16) . . ?
C4 N1 Re1 132.66(19) . . ?
C4 N1 C8 116.3(2) . . ?
C8 N1 Re1 110.93(17) . . ?
O1 C1 Re1 175.8(3) . . ?
O2 C2 Re1 177.0(3) . . ?
O3 C3 Re1 179.0(3) . . ?
N1 C4 C5 123.4(3) . . ?
N1 C4 C10 118.6(2) . . ?
C5 C4 C10 118.0(2) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 H6 120.9 . . ?
C5 C6 C7 118.3(3) . . ?
C7 C6 H6 120.9 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
N1 C8 C7 123.4(3) . . ?
N1 C8 C9 117.9(2) . . ?
C7 C8 C9 118.6(2) . . ?
O5 C9 O6 124.8(3) . . ?
O5 C9 C8 119.7(3) . . ?
O6 C9 C8 115.4(2) . . ?
F1 C10 F2 107.5(2) . . ?
F1 C10 F3 106.7(2) . . ?
F1 C10 C4 112.6(2) . . ?
F2 C10 C4 111.6(2) . . ?
F3 C10 F2 106.8(3) . . ?
F3 C10 C4 111.3(2) . . ?

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
O4 H4A O5 0.83(4) 1.84(4) 2.669(3) 175(4) 1_545 yes
O4 H4B O6 0.91(4) 1.77(5) 2.679(3) 177(4) 3_666 yes

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
Re1 O6 C9 O5 -179.8(2) . . . . ?
Re1 O6 C9 C8 0.2(3) . . . . ?
Re1 N1 C4 C5 -175.1(2) . . . . ?
Re1 N1 C4 C10 4.4(4) . . . . ?
Re1 N1 C8 C7 173.6(2) . . . . ?
Re1 N1 C8 C9 -9.3(3) . . . . ?
N1 C4 C5 C6 2.0(4) . . . . ?
N1 C4 C10 F1 53.2(3) . . . . ?
N1 C4 C10 F2 -67.8(3) . . . . ?
N1 C4 C10 F3 172.9(3) . . . . ?
N1 C8 C9 O5 -173.4(2) . . . . ?
N1 C8 C9 O6 6.6(3) . . . . ?
C4 N1 C8 C7 -3.8(4) . . . . ?
C4 N1 C8 C9 173.3(2) . . . . ?
C4 C5 C6 C7 -3.4(4) . . . . ?
C5 C4 C10 F1 -127.2(3) . . . . ?
C5 C4 C10 F2 111.7(3) . . . . ?
C5 C4 C10 F3 -7.5(4) . . . . ?
C5 C6 C7 C8 1.3(5) . . . . ?
C6 C7 C8 N1 2.4(4) . . . . ?
C6 C7 C8 C9 -174.7(3) . . . . ?
C7 C8 C9 O5 3.9(4) . . . . ?
C7 C8 C9 O6 -176.1(2) . . . . ?
C8 N1 C4 C5 1.6(4) . . . . ?
C8 N1 C4 C10 -178.9(2) . . . . ?
C10 C4 C5 C6 -177.5(3) . . . . ?

####################################################################### 
# 
# 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_37
_database_code_depnum_ccdc_archive 'CCDC 2205526'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-08-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H6 N O8 Re'
_chemical_formula_sum            'C10 H6 N O8 Re'
_chemical_formula_weight         454.36
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.54130(10)
_cell_length_b                   6.84780(10)
_cell_length_c                   17.1068(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.5150(10)
_cell_angle_gamma                90
_cell_volume                     1200.65(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14601
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.1640
_cell_measurement_theta_min      2.6200
_shelx_estimated_absorpt_T_max   0.214
_shelx_estimated_absorpt_T_min   0.081
_exptl_absorpt_coefficient_mu    20.225
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             848
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 5 0.0548
2 0 -5 0.0558
5 -1 4 0.1086
-1 0 0 0.0926
0 -1 0 0.0853
-1 4 -3 0.0753
1 1 0 0.1001
-1 -1 0 0.1060

_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11

_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.430
_diffrn_reflns_theta_min         4.314
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -7.00   0.80    1.00    --  -42.49 125.00 120.00  100
  2  ω    -21.00  72.60   0.80    1.00    --   42.49 -77.00 -30.00  117
  3  ω     20.00 113.60   0.80    1.00    --   42.49  37.00  90.00  117
  4  ω     16.00 112.00   0.80    1.00    --   42.49  57.00 120.00  120
  5  ω     87.00 176.60   0.80    4.00    --  111.00  30.00   0.00  112
  6  ω     30.00 106.00   0.80    4.00    --  111.00 -94.00 -60.00   95
  7  ω     37.00 141.00   0.80    4.00    --  111.00 -77.00 150.00  130
  8  ω     87.00 176.60   0.80    4.00    --  111.00  30.00-120.00  112
  9  ω     30.00 106.00   0.80    4.00    --  111.00 -94.00 150.00   95
 10  ω     36.00 108.00   0.80    4.00    --  111.00-111.00  30.00   90
 11  ω     36.00 108.00   0.80    4.00    --  111.00-111.00  60.00   90
 12  ω     36.00 108.00   0.80    4.00    --  111.00-111.00 120.00   90
 13  ω     36.00 108.00   0.80    4.00    --  111.00-111.00   0.00   90
 14  ω    104.00 176.80   0.80    4.00    --  111.00 111.00-120.00   91
 15  ω     24.00 176.80   0.80    4.00    --  111.00   0.00   0.00  191
 16  ω     16.00 112.00   0.80    1.00    --   42.49  57.00-180.00  120
 17  ω    -30.00  63.60   0.80    1.00    --   42.49 -37.00   0.00  117
 18  ω     16.00 112.00   0.80    1.00    --   42.49  57.00-120.00  120
 19  ω     16.00 112.00   0.80    1.00    --   42.49  57.00 -30.00  120
 20  ω     83.00 176.60   0.80    4.00    --  111.00  61.00  30.00  117
 21  ω     87.00 176.60   0.80    4.00    --  111.00  45.00-180.00  112
 22  ω     66.00 178.00   0.80    4.00    --  111.00  15.00 150.00  140
 23  ω     83.00 156.60   0.80    4.00    --  111.00  61.00 -90.00   92
 24  ω     83.00 176.60   0.80    4.00    --  111.00  61.00  60.00  117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292139000
_diffrn_orient_matrix_UB_12      -0.2168429000
_diffrn_orient_matrix_UB_13      -0.0124768000
_diffrn_orient_matrix_UB_21      -0.1470706000
_diffrn_orient_matrix_UB_22      -0.0399068000
_diffrn_orient_matrix_UB_23      -0.0310016000
_diffrn_orient_matrix_UB_31      0.0105880000
_diffrn_orient_matrix_UB_32      0.0455781000
_diffrn_orient_matrix_UB_33      -0.0863487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2456
_reflns_number_total             2457

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00248(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0255P)²+4.5954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0595
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O4-H4A = O4-H4B = O8-H8
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.2005(4) 0.8967(6) 0.4549(3) 0.0154(8) Uani 1 1 d . . . . .
C2 C 0.3221(4) 0.6772(7) 0.5742(3) 0.0190(8) Uani 1 1 d . . . . .
C3 C 0.3934(5) 1.0468(6) 0.5694(3) 0.0192(8) Uani 1 1 d . . . . .
C4 C 0.3114(4) 0.9122(5) 0.7633(3) 0.0122(8) Uani 1 1 d . . . . .
C5 C 0.3109(4) 0.9790(6) 0.8402(2) 0.0153(7) Uani 1 1 d . . . . .
H5 H 0.363613 0.917292 0.886201 0.018 Uiso 1 1 calc R U . . .
C6 C 0.2330(4) 1.1356(7) 0.8487(3) 0.0184(8) Uani 1 1 d . . . . .
H6 H 0.228295 1.180520 0.900505 0.022 Uiso 1 1 calc R U . . .
C7 C 0.1613(4) 1.2265(6) 0.7795(3) 0.0168(8) Uani 1 1 d . . . . .
H7 H 0.107096 1.335139 0.783344 0.020 Uiso 1 1 calc R U . . .
C8 C 0.1701(3) 1.1568(6) 0.7055(2) 0.0117(7) Uani 1 1 d . . . . .
C9 C 0.1041(4) 1.2622(6) 0.6294(2) 0.0126(7) Uani 1 1 d . . . . .
C10 C 0.3981(4) 0.7455(6) 0.7539(2) 0.0123(7) Uani 1 1 d . . . . .
N1 N 0.2419(3) 0.9973(5) 0.6961(2) 0.0110(6) Uani 1 1 d . . . . .
O1 O 0.1824(3) 0.8895(5) 0.38675(19) 0.0220(7) Uani 1 1 d . . . . .
O2 O 0.3731(4) 0.5292(5) 0.5731(2) 0.0331(8) Uani 1 1 d . . . . .
O3 O 0.4910(3) 1.1187(5) 0.5701(2) 0.0270(7) Uani 1 1 d . . . . .
O4 O 0.0465(3) 0.7857(4) 0.57944(17) 0.0139(5) Uani 1 1 d D . . . .
O5 O 0.0468(3) 1.4155(4) 0.6329(2) 0.0199(6) Uani 1 1 d . . . . .
O6 O 0.1163(3) 1.1786(4) 0.56371(17) 0.0158(6) Uani 1 1 d . . . . .
O7 O 0.5123(3) 0.7682(4) 0.75286(19) 0.0178(6) Uani 1 1 d . . . . .
O8 O 0.3406(3) 0.5757(4) 0.7494(2) 0.0191(6) Uani 1 1 d D . . . .
Re1 Re 0.23192(2) 0.91997(2) 0.56992(2) 0.01105(10) Uani 1 1 d . . . . .
H4A H -0.004(5) 0.788(10) 0.5349(18) 0.037(17) Uiso 1 1 d D . . . .
H4B H 0.060(7) 0.677(5) 0.600(4) 0.05(2) Uiso 1 1 d D . . . .
H8 H 0.391(6) 0.490(8) 0.742(5) 0.05(2) Uiso 1 1 d 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
C1 O1 1.138(6) . ?
C1 Re1 1.924(4) . ?
C2 O2 1.149(6) . ?
C2 Re1 1.908(4) . ?
C3 O3 1.138(6) . ?
C3 Re1 1.913(5) . ?
C4 C5 1.394(6) . ?
C4 C10 1.495(5) . ?
C4 N1 1.343(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.393(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(6) . ?
C8 C9 1.508(5) . ?
C8 N1 1.360(5) . ?
C9 O5 1.219(5) . ?
C9 O6 1.295(5) . ?
C10 O7 1.218(5) . ?
C10 O8 1.305(5) . ?
N1 Re1 2.202(3) . ?
O4 Re1 2.200(3) . ?
O4 H4A 0.820(10) . ?
O4 H4B 0.821(10) . ?
O6 Re1 2.138(3) . ?
O8 H8 0.818(10) . ?

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
O1 C1 Re1 177.7(4) . . ?
O2 C2 Re1 176.8(4) . . ?
O3 C3 Re1 178.3(4) . . ?
C5 C4 C10 119.3(4) . . ?
N1 C4 C5 122.9(4) . . ?
N1 C4 C10 117.7(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 H6 120.8 . . ?
C5 C6 C7 118.4(4) . . ?
C7 C6 H6 120.8 . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(4) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 120.8(4) . . ?
N1 C8 C7 123.1(4) . . ?
N1 C8 C9 116.1(3) . . ?
O5 C9 C8 120.3(4) . . ?
O5 C9 O6 125.0(4) . . ?
O6 C9 C8 114.7(3) . . ?
O7 C10 C4 122.4(4) . . ?
O7 C10 O8 124.1(4) . . ?
O8 C10 C4 113.5(3) . . ?
C4 N1 C8 117.1(3) . . ?
C4 N1 Re1 128.8(3) . . ?
C8 N1 Re1 114.1(2) . . ?
Re1 O4 H4A 108(5) . . ?
Re1 O4 H4B 110(5) . . ?
H4A O4 H4B 115(7) . . ?
C9 O6 Re1 119.6(2) . . ?
C10 O8 H8 110(6) . . ?
C1 Re1 N1 168.57(14) . . ?
C1 Re1 O4 95.60(14) . . ?
C1 Re1 O6 93.31(14) . . ?
C2 Re1 C1 86.11(17) . . ?
C2 Re1 C3 87.70(19) . . ?
C2 Re1 N1 105.24(15) . . ?
C2 Re1 O4 94.39(15) . . ?
C2 Re1 O6 175.31(15) . . ?
C3 Re1 C1 88.49(18) . . ?
C3 Re1 N1 93.26(15) . . ?
C3 Re1 O4 175.52(14) . . ?
C3 Re1 O6 96.94(15) . . ?
O4 Re1 N1 82.38(11) . . ?
O6 Re1 N1 75.26(11) . . ?
O6 Re1 O4 81.03(11) . . ?

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
C7 H7 O1 0.95 2.58 3.185(5) 121.7 4_586 yes
O4 H4A O6 0.820(10) 1.836(13) 2.653(4) 174(7) 3_576 yes
O4 H4B O5 0.821(10) 1.89(2) 2.695(4) 166(7) 1_545 yes
O8 H8 O7 0.818(10) 1.82(2) 2.620(4) 165(8) 2_646 yes

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
C4 C5 C6 C7 -2.6(6) . . . . ?
C5 C4 C10 O7 -84.6(5) . . . . ?
C5 C4 C10 O8 93.4(4) . . . . ?
C5 C4 N1 C8 0.9(6) . . . . ?
C5 C4 N1 Re1 178.6(3) . . . . ?
C5 C6 C7 C8 0.3(6) . . . . ?
C6 C7 C8 C9 -174.3(4) . . . . ?
C6 C7 C8 N1 2.7(6) . . . . ?
C7 C8 C9 O5 3.2(6) . . . . ?
C7 C8 C9 O6 -177.9(4) . . . . ?
C7 C8 N1 C4 -3.3(5) . . . . ?
C7 C8 N1 Re1 178.7(3) . . . . ?
C8 C9 O6 Re1 -3.1(4) . . . . ?
C9 C8 N1 C4 173.8(3) . . . . ?
C9 C8 N1 Re1 -4.2(4) . . . . ?
C10 C4 C5 C6 178.5(4) . . . . ?
C10 C4 N1 C8 -175.7(3) . . . . ?
C10 C4 N1 Re1 2.0(5) . . . . ?
N1 C4 C5 C6 2.0(6) . . . . ?
N1 C4 C10 O7 92.1(5) . . . . ?
N1 C4 C10 O8 -89.9(4) . . . . ?
N1 C8 C9 O5 -174.0(3) . . . . ?
N1 C8 C9 O6 4.9(5) . . . . ?
O5 C9 O6 Re1 175.7(3) . . . . ?


####################################################################### 
# 
# 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_29
_database_code_depnum_ccdc_archive 'CCDC 2205517'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O7 Re, H2 O'
_chemical_formula_sum            'C10 H10 N O8 Re'
_chemical_formula_weight         458.39
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.61350(10)
_cell_length_b                   11.21590(10)
_cell_length_c                   9.56510(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.0710(10)
_cell_angle_gamma                90
_cell_volume                     2633.90(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    22994
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3870
_cell_measurement_theta_min      3.5470
_shelx_estimated_absorpt_T_max   0.608
_shelx_estimated_absorpt_T_min   0.288
_exptl_absorpt_coefficient_mu    18.440
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0452
0 1 0 0.0452
-1 0 0 0.0144
1 0 0 0.0144
0 -1 1 0.0289
0 1 -1 0.0509
-1 1 1 0.0357
1 -1 -1 0.0357

_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03

_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0060
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25893
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.460
_diffrn_reflns_theta_min         3.601
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -20.00   0.80    6.00    --  -42.61 -37.00 -90.00  120
  2  ω    -80.00  36.00   0.80    6.00    --  -42.61  19.00  90.00  145
  3  ω    -87.00  -7.00   0.80    6.00    --  -42.61 125.00  60.00  100
  4  ω     11.00  40.60   0.80    6.00    --   42.61  76.00  42.92   37
  5  ω     10.00  42.00   0.80    6.00    --   42.61  81.00   8.77   40
  6  ω      6.00  82.00   0.80    6.00    --   42.61 -99.00 150.00   95
  7  ω     10.00  42.00   0.80    6.00    --   42.61  82.00-139.83   40
  8  ω     11.00  40.60   0.80    6.00    --   42.61  79.00-102.24   37
  9  ω     11.00  40.60   0.80    6.00    --   42.61  79.00 -79.18   37
 10  ω     30.00 106.00   0.80   24.00    --  111.00 -94.00 120.00   95
 11  ω    104.00 177.60   0.80   24.00    --  111.00 111.00  90.00   92
 12  ω     36.00 134.40   0.80   24.00    --  111.00 -30.00 120.00  123
 13  ω     30.00 106.00   0.80   24.00    --  111.00 -94.00   0.00   95
 14  ω    104.00 177.60   0.80   24.00    --  111.00 111.00  30.00   92
 15  ω     30.00 106.00   0.80   24.00    --  111.00 -94.00 -30.00   95
 16  ω     81.00 177.00   0.80   24.00    --  111.00  71.00 -91.50  120
 17  ω     30.00 106.00   0.80   24.00    --  111.00 -94.00  30.00   95
 18  ω     61.00 145.00   0.80   24.00    --  111.00 178.00-180.00  105
 19  ω    104.00 177.60   0.80   24.00    --  111.00 111.00 -60.00   92
 20  ω     41.00 126.60   0.80   24.00    --  111.00-144.00  96.30  107
 21  ω     36.00 108.00   0.80   24.00    --  111.00-111.00 -30.00   90
 22  ω     81.00 177.00   0.80   24.00    --  111.00  70.00 131.91  120
 23  ω     36.00 108.00   0.80   24.00    --  111.00-111.00 120.00   90
 24  ω    104.00 177.60   0.80   24.00    --  111.00 111.00-180.00   92
 25  ω     61.00 145.00   0.80   24.00    --  111.00 178.00 -60.00  105
 26  ω     37.00 141.00   0.80   24.00    --  111.00 -77.00-120.00  130
 27  ω    103.00 177.40   0.80   24.00    --  111.00  77.00-150.00   93
 28  ω     36.00 108.00   0.80   24.00    --  111.00-111.00-120.00   90
 29  ω     36.00 108.00   0.80   24.00    --  111.00-111.00  90.00   90
 30  ω     36.00 108.00   0.80   24.00    --  111.00-111.00 -60.00   90
 31  ω     83.00 177.40   0.80   24.00    --  111.00  62.00 163.87  118
 32  ω    104.00 177.60   0.80   24.00    --  111.00 111.00  60.00   92
 33  ω     36.00 108.00   0.80   24.00    --  111.00-111.00-180.00   90
 34  ω     36.00 108.00   0.80   24.00    --  111.00-111.00  60.00   90
 35  ω     34.00 106.80   0.80   24.00    --  111.00-106.00-109.36   91
 36  ω   -113.00 -17.00   0.80    6.00    --  -42.61 -57.00-180.00  120
 37  ω   -116.00 -20.00   0.80    6.00    --  -42.61 -37.00  60.00  120
 38  ω   -114.00 -19.60   0.80    6.00    --  -42.61 -42.00 -13.00  118
 39  ω     11.00  40.60   0.80    6.00    --   42.61  78.00 178.69   37
 40  ω     11.00  40.60   0.80    6.00    --   42.61  77.00 -44.49   37
 41  ω      6.00  82.00   0.80    6.00    --   42.61 -99.00 -60.00   95
 42  ω    -30.00  64.40   0.80    6.00    --   42.61 -37.00 150.00  118
 43  ω     11.00  40.60   0.80    6.00    --   42.61  78.00 116.87   37
 44  ω     66.00 178.00   0.80   24.00    --  111.00  15.00  30.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0124446000
_diffrn_orient_matrix_UB_12      -0.0256650000
_diffrn_orient_matrix_UB_13      -0.1527413000
_diffrn_orient_matrix_UB_21      -0.0383838000
_diffrn_orient_matrix_UB_22      -0.1086061000
_diffrn_orient_matrix_UB_23      -0.0026069000
_diffrn_orient_matrix_UB_31      -0.0480318000
_diffrn_orient_matrix_UB_32      0.0800832000
_diffrn_orient_matrix_UB_33      -0.0524157000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2683
_reflns_number_total             2686

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.000273(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2686
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0123
_refine_ls_R_factor_gt           0.0123
_refine_ls_restrained_S_all      1.215
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+4.7315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0309
_refine_ls_wR_factor_ref         0.0309
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All H(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 O8-H8A = O8-H8C
 0.82 with sigma of 0.01
 O8-H8B
 0.82 with sigma of 0.01
3. Others
 Fixed Sof: H8B(0.5) H8C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.61996(9) 0.0016(2) 0.4069(2) 0.0246(4) Uani 1 1 d . . . . .
C2 C 0.68243(10) 0.16715(18) 0.5417(3) 0.0250(5) Uani 1 1 d . . . . .
C3 C 0.68621(9) 0.13533(19) 0.2712(2) 0.0250(4) Uani 1 1 d . . . . .
C4 C 0.65775(8) 0.44305(17) 0.4297(2) 0.0168(4) Uani 1 1 d . . . . .
H4 H 0.683892 0.415417 0.500137 0.020 Uiso 1 1 calc R U . . .
C5 C 0.65204(8) 0.56487(18) 0.4066(2) 0.0198(4) Uani 1 1 d . . . . .
C6 C 0.61383(9) 0.60526(19) 0.3023(2) 0.0239(4) Uani 1 1 d . . . . .
H6 H 0.609394 0.688127 0.284393 0.029 Uiso 1 1 calc R U . . .
C7 C 0.58263(8) 0.52256(18) 0.2259(2) 0.0226(4) Uani 1 1 d . . . . .
H7 H 0.556278 0.547720 0.154594 0.027 Uiso 1 1 calc R U . . .
C8 C 0.59027(8) 0.40205(17) 0.2545(2) 0.0177(4) Uani 1 1 d . . . . .
C9 C 0.55706(8) 0.30667(18) 0.1786(2) 0.0186(4) Uani 1 1 d . . . . .
C10 C 0.72336(9) 0.6078(2) 0.5803(2) 0.0246(4) Uani 1 1 d . . . . .
H10A H 0.747676 0.553175 0.534775 0.037 Uiso 1 1 calc R U . . .
H10B H 0.706712 0.566076 0.656550 0.037 Uiso 1 1 calc R U . . .
H10C H 0.744285 0.676191 0.618474 0.037 Uiso 1 1 calc R U . . .
N1 N 0.62709(6) 0.36354(15) 0.35457(17) 0.0163(3) Uani 1 1 d . . . . .
O1 O 0.61482(8) -0.09959(15) 0.4155(2) 0.0399(4) Uani 1 1 d . . . . .
O2 O 0.71583(8) 0.16839(16) 0.6313(2) 0.0405(5) Uani 1 1 d . . . . .
O3 O 0.72141(7) 0.10944(16) 0.2052(2) 0.0375(4) Uani 1 1 d . . . . .
O4 O 0.56343(6) 0.21683(13) 0.52193(15) 0.0197(3) Uani 1 1 d . . . . .
H4A H 0.5370(13) 0.248(3) 0.482(3) 0.037(8) Uiso 1 1 d . . . . .
H4B H 0.5541(13) 0.157(3) 0.565(4) 0.040(9) Uiso 1 1 d . . . . .
H8B H 0.507(3) 0.008(8) 0.557(5) 0.060 Uiso 0.5 1 d D U P A 1
H8C H 0.512(3) 0.022(6) 0.703(5) 0.060 Uiso 0.5 1 d D U P B 2
H8A H 0.5420(14) -0.0507(18) 0.647(4) 0.060 Uiso 1 1 d D U . . .
O5 O 0.52262(7) 0.33413(13) 0.08504(17) 0.0253(3) Uani 1 1 d . . . . .
O6 O 0.56745(6) 0.19951(13) 0.22147(15) 0.0205(3) Uani 1 1 d . . . . .
O7 O 0.68150(6) 0.64861(13) 0.47970(17) 0.0253(3) Uani 1 1 d . . . . .
O8 O 0.52710(7) 0.01347(14) 0.62961(17) 0.0261(3) Uani 1 1 d D . . . .
Re1 Re 0.62897(2) 0.17124(2) 0.38818(2) 0.01592(5) 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
C1 O1 1.146(3) . ?
C1 Re1 1.925(2) . ?
C2 O2 1.145(3) . ?
C2 Re1 1.901(2) . ?
C3 O3 1.145(3) . ?
C3 Re1 1.903(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C4 N1 1.343(2) . ?
C5 C6 1.397(3) . ?
C5 O7 1.351(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.380(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(3) . ?
C8 C9 1.502(3) . ?
C8 N1 1.342(3) . ?
C9 O5 1.227(3) . ?
C9 O6 1.290(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 O7 1.434(3) . ?
N1 Re1 2.1806(17) . ?
O4 H4A 0.81(3) . ?
O4 H4B 0.82(3) . ?
O4 Re1 2.1893(14) . ?
O6 Re1 2.1432(14) . ?
O8 H8B 0.820(10) . ?
O8 H8C 0.821(10) . ?
O8 H8A 0.820(10) . ?

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
O1 C1 Re1 178.7(2) . . ?
O2 C2 Re1 177.1(2) . . ?
O3 C3 Re1 176.7(2) . . ?
C5 C4 H4 119.3 . . ?
N1 C4 H4 119.3 . . ?
N1 C4 C5 121.41(18) . . ?
C4 C5 C6 119.19(19) . . ?
O7 C5 C4 123.84(18) . . ?
O7 C5 C6 116.97(18) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 C5 118.78(19) . . ?
C7 C6 H6 120.6 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.13(19) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 122.41(18) . . ?
N1 C8 C7 121.94(18) . . ?
N1 C8 C9 115.63(17) . . ?
O5 C9 C8 119.86(18) . . ?
O5 C9 O6 125.24(19) . . ?
O6 C9 C8 114.89(17) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O7 C10 H10A 109.5 . . ?
O7 C10 H10B 109.5 . . ?
O7 C10 H10C 109.5 . . ?
C4 N1 Re1 124.93(13) . . ?
C8 N1 C4 119.54(17) . . ?
C8 N1 Re1 115.45(13) . . ?
H4A O4 H4B 110(3) . . ?
Re1 O4 H4A 115(2) . . ?
Re1 O4 H4B 110(2) . . ?
C9 O6 Re1 119.23(12) . . ?
C5 O7 C10 117.32(16) . . ?
H8B O8 H8A 110(6) . . ?
H8C O8 H8A 99(6) . . ?
C1 Re1 N1 171.79(8) . . ?
C1 Re1 O4 94.70(8) . . ?
C1 Re1 O6 97.78(7) . . ?
C2 Re1 C1 88.99(9) . . ?
C2 Re1 C3 87.03(10) . . ?
C2 Re1 N1 98.28(7) . . ?
C2 Re1 O4 93.02(8) . . ?
C2 Re1 O6 172.66(7) . . ?
C3 Re1 C1 86.59(9) . . ?
C3 Re1 N1 97.55(8) . . ?
C3 Re1 O4 178.71(7) . . ?
C3 Re1 O6 96.16(8) . . ?
N1 Re1 O4 81.16(6) . . ?
O6 Re1 N1 74.78(6) . . ?
O6 Re1 O4 83.64(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
O4 H4A O5 0.81(3) 1.84(3) 2.638(2) 171(3) 2_655 yes
O4 H4B O8 0.82(3) 1.87(3) 2.682(2) 170(3) . yes
O8 H8B O8 0.820(10) 1.937(18) 2.747(3) 169(8) 5_656 yes
O8 H8C O8 0.821(10) 1.932(17) 2.742(3) 169(7) 2_656 yes
O8 H8A O6 0.820(10) 1.902(13) 2.709(2) 168(4) 6_556 yes

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
C4 C5 C6 C7 0.4(3) . . . . ?
C4 C5 O7 C10 4.2(3) . . . . ?
C5 C4 N1 C8 0.3(3) . . . . ?
C5 C4 N1 Re1 -176.47(14) . . . . ?
C5 C6 C7 C8 -0.2(3) . . . . ?
C6 C5 O7 C10 -175.87(19) . . . . ?
C6 C7 C8 C9 178.5(2) . . . . ?
C6 C7 C8 N1 0.1(3) . . . . ?
C7 C8 C9 O5 1.8(3) . . . . ?
C7 C8 C9 O6 -177.09(19) . . . . ?
C7 C8 N1 C4 -0.1(3) . . . . ?
C7 C8 N1 Re1 176.95(16) . . . . ?
C8 C9 O6 Re1 -0.6(2) . . . . ?
C9 C8 N1 C4 -178.62(17) . . . . ?
C9 C8 N1 Re1 -1.6(2) . . . . ?
N1 C4 C5 C6 -0.4(3) . . . . ?
N1 C4 C5 O7 179.51(18) . . . . ?
N1 C8 C9 O5 -179.66(19) . . . . ?
N1 C8 C9 O6 1.4(3) . . . . ?
O5 C9 O6 Re1 -179.41(17) . . . . ?
O7 C5 C6 C7 -179.6(2) . . . . ?


####################################################################### 
# 
# 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_22
_database_code_depnum_ccdc_archive 'CCDC 2205516'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C9 H5 F N O6 Re), C H4 O'
_chemical_formula_sum            'C19 H14 F2 N2 O13 Re2'
_chemical_formula_weight         888.72
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7973(2)
_cell_length_b                   10.6398(3)
_cell_length_c                   12.7440(3)
_cell_angle_alpha                78.502(2)
_cell_angle_beta                 68.184(2)
_cell_angle_gamma                73.235(2)
_cell_volume                     1174.53(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18850
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.9540
_cell_measurement_theta_min      3.6970
_shelx_estimated_absorpt_T_max   0.683
_shelx_estimated_absorpt_T_min   0.098
_exptl_absorpt_coefficient_mu    20.674
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             828
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0291
-1 0 -1 0.0211
0 -1 5 0.0798
0 1 -5 0.0798
0 -1 0 0.0143
0 1 0 0.0013

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02

_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24608
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.450
_diffrn_reflns_theta_min         3.756
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     29.00 125.00   0.50    0.10    --   51.79  77.00 -30.00  192
  2  ω     92.00 178.00   0.50    0.20    --  107.75  61.00-120.00  172
  3  ω     96.00 178.00   0.50    0.20    --  107.75  15.00 -30.00  164
  4  ω     94.00 137.00   0.50    0.20    --  107.75  30.00 150.00   86
  5  ω     96.00 178.00   0.50    0.20    --  107.75  15.00  60.00  164
  6  ω   -124.00 -37.00   0.50    0.10    --  -51.79 -57.00 -90.00  174
  7  ω   -125.00 -29.00   0.50    0.10    --  -51.79 -77.00   0.00  192
  8  ω   -125.00 -29.00   0.50    0.10    --  -51.79 -77.00  60.00  192
  9  ω   -125.00 -29.00   0.50    0.10    --  -51.79 -77.00 150.00  192
 10  ω    -83.00  -2.00   0.50    0.10    --  -51.79 112.00 -69.00  162
 11  ω    -83.00 -10.00   0.50    0.20    --  -86.25 112.00 -69.00  146
 12  ω   -157.00 -70.00   0.50    0.20    --  -86.25 -61.00  90.00  174
 13  ω   -124.00 -37.00   0.50    0.10    --  -51.79 -57.00  90.00  174
 14  ω   -159.00 -64.00   0.50    0.20    --  -86.25 -76.00 -84.16  190
 15  ω   -156.00 -69.00   0.50    0.20    --  -86.25 -64.00-151.73  174
 16  ω   -124.00 -37.00   0.50    0.10    --  -51.79 -57.00-180.00  174
 17  ω   -128.00 -80.00   0.50    0.10    --  -51.79-112.00-162.00   96
 18  ω   -162.00 -80.00   0.50    0.20    --  -86.25-112.00-162.00  164
 19  ω   -126.00 -73.00   0.50    0.10    --  -51.79-125.00  30.00  106
 20  ω     62.00 146.00   0.50    0.20    --  107.75 178.00  30.00  168
 21  ω    102.00 178.00   0.50    0.20    --  107.75 111.00 -30.00  152
 22  ω    102.00 178.00   0.50    0.20    --  107.75 111.00 -90.00  152
 23  ω    102.00 178.00   0.50    0.20    --  107.75 111.00-180.00  152
 24  ω    102.00 178.00   0.50    0.20    --  107.75 112.00 -69.00  152
 25  ω    102.00 178.00   0.50    0.20    --  107.75 111.00  90.00  152
 26  ω     37.00 124.00   0.50    0.20    --  107.75 -61.00 120.00  174
 27  ω     34.00  99.00   0.50    0.10    --   51.79-125.00  90.00  130
 28  ω     31.00 109.00   0.50    0.20    --  107.75-111.00 150.00  156
 29  ω     31.00 109.00   0.50    0.20    --  107.75-111.00 120.00  156
 30  ω     31.00 106.00   0.50    0.20    --  107.75 -94.00   0.00  150
 31  ω     24.00  93.00   0.50    0.10    --   51.79-112.00-162.00  138
 32  ω     32.00 109.00   0.50    0.20    --  107.75-112.00-162.00  154
 33  ω     31.00 109.00   0.50    0.20    --  107.75-111.00 -90.00  156
 34  ω     31.00 106.00   0.50    0.20    --  107.75 -94.00 -90.00  150
 35  ω     31.00 106.00   0.50    0.20    --  107.75 -94.00  30.00  150
 36  ω     31.00 106.00   0.50    0.20    --  107.75 -94.00  60.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0245998000
_diffrn_orient_matrix_UB_12      -0.1426735000
_diffrn_orient_matrix_UB_13      0.0572852000
_diffrn_orient_matrix_UB_21      -0.0412771000
_diffrn_orient_matrix_UB_22      0.0524268000
_diffrn_orient_matrix_UB_23      0.1148763000
_diffrn_orient_matrix_UB_31      -0.1675255000
_diffrn_orient_matrix_UB_32      0.0034024000
_diffrn_orient_matrix_UB_33      0.0257045000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4468
_reflns_number_total             4747

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.174
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0191
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²+1.9020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0495
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C13(H13), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.23255(2) 0.76799(2) 0.60164(2) 0.01815(6) Uani 1 1 d . . . . .
F1 F 0.5659(3) 0.5351(3) 0.8820(2) 0.0495(6) Uani 1 1 d . . . . .
O1 O -0.0107(3) 0.8592(3) 0.4875(3) 0.0367(6) Uani 1 1 d . . . . .
O2 O 0.0087(3) 0.6284(3) 0.7905(2) 0.0309(6) Uani 1 1 d . . . . .
O3 O 0.3263(3) 0.5066(3) 0.5015(2) 0.0354(6) Uani 1 1 d . . . . .
O4 O 0.1725(3) 0.9499(2) 0.6810(2) 0.0228(5) Uani 1 1 d . . . . .
H4A H 0.235(6) 0.996(5) 0.649(4) 0.040(13) Uiso 1 1 d . . . . .
H4B H 0.159(6) 0.931(5) 0.751(5) 0.046(14) Uiso 1 1 d . . . . .
O5 O 0.6335(3) 0.8844(3) 0.4132(2) 0.0362(6) Uani 1 1 d . . . . .
O6 O 0.3962(3) 0.8636(2) 0.4757(2) 0.0245(5) Uani 1 1 d . . . . .
N1 N 0.4236(3) 0.7182(3) 0.6634(2) 0.0207(6) Uani 1 1 d . . . . .
C1 C 0.0797(4) 0.8268(3) 0.5311(3) 0.0253(7) Uani 1 1 d . . . . .
C2 C 0.0928(4) 0.6844(3) 0.7223(3) 0.0232(7) Uani 1 1 d . . . . .
C3 C 0.2942(4) 0.6063(4) 0.5358(3) 0.0251(7) Uani 1 1 d . . . . .
C4 C 0.4316(4) 0.6449(3) 0.7599(3) 0.0254(7) Uani 1 1 d . . . . .
H4 H 0.345582 0.615154 0.811722 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5634(5) 0.6120(4) 0.7850(4) 0.0339(9) Uani 1 1 d . . . . .
C6 C 0.6896(5) 0.6551(4) 0.7135(4) 0.0380(9) Uani 1 1 d . . . . .
H6 H 0.780296 0.632462 0.731128 0.046 Uiso 1 1 calc R U . . .
C7 C 0.6787(4) 0.7324(4) 0.6155(3) 0.0307(8) Uani 1 1 d . . . . .
H7 H 0.762559 0.765501 0.564138 0.037 Uiso 1 1 calc R U . . .
C8 C 0.5464(4) 0.7620(3) 0.5916(3) 0.0231(7) Uani 1 1 d . . . . .
C9 C 0.5281(4) 0.8430(3) 0.4844(3) 0.0240(7) Uani 1 1 d . . . . .
Re2 Re 0.25983(2) 0.24198(2) 0.91736(2) 0.01711(6) Uani 1 1 d . . . . .
F2 F -0.0207(3) 0.3978(2) 0.59685(19) 0.0403(5) Uani 1 1 d . . . . .
O7 O 0.4894(3) 0.1950(3) 1.0397(3) 0.0411(7) Uani 1 1 d . . . . .
O8 O 0.5001(3) 0.3418(3) 0.7106(2) 0.0351(6) Uani 1 1 d . . . . .
O9 O 0.1598(3) 0.5210(2) 0.9877(2) 0.0304(6) Uani 1 1 d . . . . .
O10 O 0.3269(3) 0.0457(3) 0.8675(3) 0.0365(7) Uani 1 1 d . . . . .
O11 O -0.1369(3) 0.1119(3) 1.0945(2) 0.0272(5) Uani 1 1 d . . . . .
O12 O 0.0865(3) 0.1585(2) 1.0468(2) 0.0213(5) Uani 1 1 d . . . . .
N2 N 0.0862(3) 0.2652(3) 0.8420(2) 0.0192(6) Uani 1 1 d . . . . .
C10 C 0.4020(4) 0.2099(4) 0.9954(3) 0.0266(8) Uani 1 1 d . . . . .
C11 C 0.4093(4) 0.3038(3) 0.7879(3) 0.0251(7) Uani 1 1 d . . . . .
C12 C 0.1934(4) 0.4162(3) 0.9627(3) 0.0212(7) Uani 1 1 d . . . . .
C13 C 0.0905(4) 0.3227(3) 0.7376(3) 0.0230(7) Uani 1 1 d . . . . .
H13 H 0.176176 0.354973 0.688742 0.028 Uiso 1 1 calc R U . . .
C14 C -0.0291(4) 0.3353(4) 0.7008(3) 0.0297(8) Uani 1 1 d . . . . .
C15 C -0.1540(4) 0.2887(4) 0.7678(3) 0.0331(8) Uani 1 1 d . . . . .
H15 H -0.235868 0.297552 0.741873 0.040 Uiso 1 1 calc R U . . .
C16 C -0.1557(4) 0.2279(4) 0.8751(3) 0.0278(8) Uani 1 1 d . . . . .
H16 H -0.239530 0.193363 0.924464 0.033 Uiso 1 1 calc R U . . .
C17 C -0.0361(4) 0.2179(3) 0.9094(3) 0.0198(6) Uani 1 1 d . . . . .
C18 C -0.0295(4) 0.1578(3) 1.0258(3) 0.0193(6) Uani 1 1 d . . . . .
O13 O 0.6011(3) -0.0077(3) 0.7290(2) 0.0370(6) Uani 1 1 d . . . . .
H13A H 0.597(7) 0.038(6) 0.666(5) 0.08(2) Uiso 1 1 d . . . . .
C19 C 0.7337(5) -0.0140(5) 0.7575(4) 0.0489(12) Uani 1 1 d . . . . .
H19A H 0.798123 0.038386 0.698187 0.073 Uiso 1 1 calc R U . . .
H19B H 0.790623 -0.106004 0.762932 0.073 Uiso 1 1 calc R U . . .
H19C H 0.701825 0.021283 0.830508 0.073 Uiso 1 1 calc R U . . .
H10A H 0.277(8) 0.000(6) 0.885(5) 0.073 Uiso 1 1 d . U . . .
H10B H 0.406(7) 0.020(6) 0.829(5) 0.073 Uiso 1 1 d . 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 O4 2.190(2) . ?
Re1 O6 2.135(2) . ?
Re1 N1 2.182(3) . ?
Re1 C1 1.918(4) . ?
Re1 C2 1.903(4) . ?
Re1 C3 1.905(4) . ?
F1 C5 1.344(5) . ?
O1 C1 1.151(5) . ?
O2 C2 1.155(4) . ?
O3 C3 1.142(4) . ?
O4 H4A 0.83(5) . ?
O4 H4B 0.84(5) . ?
O5 C9 1.220(4) . ?
O6 C9 1.289(5) . ?
N1 C4 1.335(5) . ?
N1 C8 1.355(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.376(5) . ?
C5 C6 1.375(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.374(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.375(5) . ?
C8 C9 1.506(5) . ?
Re2 O10 2.151(3) . ?
Re2 O12 2.145(2) . ?
Re2 N2 2.180(3) . ?
Re2 C10 1.915(4) . ?
Re2 C11 1.904(4) . ?
Re2 C12 1.909(3) . ?
F2 C14 1.343(4) . ?
O7 C10 1.150(5) . ?
O8 C11 1.150(5) . ?
O9 C12 1.142(4) . ?
O10 H10A 0.73(7) . ?
O10 H10B 0.75(6) . ?
O11 C18 1.246(4) . ?
O12 C18 1.263(4) . ?
N2 C13 1.339(4) . ?
N2 C17 1.356(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(5) . ?
C14 C15 1.369(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.366(5) . ?
C17 C18 1.511(5) . ?
O13 H13A 0.86(6) . ?
O13 C19 1.454(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
O6 Re1 O4 81.84(9) . . ?
O6 Re1 N1 75.26(10) . . ?
N1 Re1 O4 83.59(10) . . ?
C1 Re1 O4 94.74(12) . . ?
C1 Re1 O6 96.96(12) . . ?
C1 Re1 N1 172.19(12) . . ?
C2 Re1 O4 95.63(12) . . ?
C2 Re1 O6 175.57(12) . . ?
C2 Re1 N1 100.89(13) . . ?
C2 Re1 C1 86.85(15) . . ?
C2 Re1 C3 84.79(14) . . ?
C3 Re1 O4 176.74(13) . . ?
C3 Re1 O6 97.53(12) . . ?
C3 Re1 N1 93.16(13) . . ?
C3 Re1 C1 88.51(15) . . ?
Re1 O4 H4A 112(3) . . ?
Re1 O4 H4B 109(3) . . ?
H4A O4 H4B 112(5) . . ?
C9 O6 Re1 119.0(2) . . ?
C4 N1 Re1 126.2(2) . . ?
C4 N1 C8 118.9(3) . . ?
C8 N1 Re1 114.8(2) . . ?
O1 C1 Re1 178.3(3) . . ?
O2 C2 Re1 175.5(3) . . ?
O3 C3 Re1 176.4(3) . . ?
N1 C4 H4 119.7 . . ?
N1 C4 C5 120.5(3) . . ?
C5 C4 H4 119.7 . . ?
F1 C5 C4 117.8(4) . . ?
F1 C5 C6 120.5(4) . . ?
C6 C5 C4 121.6(4) . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.1(4) . . ?
C7 C6 H6 121.4 . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C8 120.0(4) . . ?
C8 C7 H7 120.0 . . ?
N1 C8 C7 121.8(3) . . ?
N1 C8 C9 115.4(3) . . ?
C7 C8 C9 122.8(3) . . ?
O5 C9 O6 124.5(4) . . ?
O5 C9 C8 120.3(3) . . ?
O6 C9 C8 115.1(3) . . ?
O10 Re2 N2 82.85(11) . . ?
O12 Re2 O10 80.32(10) . . ?
O12 Re2 N2 74.96(10) . . ?
C10 Re2 O10 95.09(14) . . ?
C10 Re2 O12 99.44(12) . . ?
C10 Re2 N2 174.27(12) . . ?
C11 Re2 O10 93.71(13) . . ?
C11 Re2 O12 171.90(12) . . ?
C11 Re2 N2 98.98(13) . . ?
C11 Re2 C10 86.47(15) . . ?
C11 Re2 C12 87.62(14) . . ?
C12 Re2 O10 178.09(12) . . ?
C12 Re2 O12 98.23(12) . . ?
C12 Re2 N2 95.59(12) . . ?
C12 Re2 C10 86.35(15) . . ?
Re2 O10 H10A 124(5) . . ?
Re2 O10 H10B 120(5) . . ?
H10A O10 H10B 116(7) . . ?
C18 O12 Re2 118.8(2) . . ?
C13 N2 Re2 125.7(2) . . ?
C13 N2 C17 118.8(3) . . ?
C17 N2 Re2 115.5(2) . . ?
O7 C10 Re2 177.3(3) . . ?
O8 C11 Re2 179.1(3) . . ?
O9 C12 Re2 177.1(3) . . ?
N2 C13 H13 119.9 . . ?
N2 C13 C14 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
F2 C14 C13 117.5(3) . . ?
F2 C14 C15 120.6(3) . . ?
C15 C14 C13 121.9(4) . . ?
C14 C15 H15 121.4 . . ?
C14 C15 C16 117.1(3) . . ?
C16 C15 H15 121.4 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.6(3) . . ?
C17 C16 H16 120.2 . . ?
N2 C17 C16 122.4(3) . . ?
N2 C17 C18 114.0(3) . . ?
C16 C17 C18 123.6(3) . . ?
O11 C18 O12 124.3(3) . . ?
O11 C18 C17 119.0(3) . . ?
O12 C18 C17 116.7(3) . . ?
C19 O13 H13A 116(4) . . ?
O13 C19 H19A 109.5 . . ?
O13 C19 H19B 109.5 . . ?
O13 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

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
O4 H4A O5 0.83(5) 1.92(5) 2.749(4) 174(5) 2_676 yes
O4 H4B O11 0.84(5) 1.88(5) 2.716(4) 178(5) 2_567 yes
O13 H13A O6 0.86(6) 1.89(6) 2.745(4) 176(6) 2_666 yes
O10 H10A O11 0.73(7) 1.98(7) 2.705(4) 169(7) 2_557 yes
O10 H10B O13 0.75(6) 1.84(6) 2.579(4) 169(7) . yes

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
Re1 O6 C9 O5 174.3(3) . . . . ?
Re1 O6 C9 C8 -5.9(4) . . . . ?
Re1 N1 C4 C5 174.8(3) . . . . ?
Re1 N1 C8 C7 -176.4(3) . . . . ?
Re1 N1 C8 C9 2.9(3) . . . . ?
F1 C5 C6 C7 179.5(3) . . . . ?
N1 C4 C5 F1 -178.4(3) . . . . ?
N1 C4 C5 C6 1.3(6) . . . . ?
N1 C8 C9 O5 -178.4(3) . . . . ?
N1 C8 C9 O6 1.8(4) . . . . ?
C4 N1 C8 C7 0.2(5) . . . . ?
C4 N1 C8 C9 179.5(3) . . . . ?
C4 C5 C6 C7 -0.2(6) . . . . ?
C5 C6 C7 C8 -0.9(5) . . . . ?
C6 C7 C8 N1 0.9(5) . . . . ?
C6 C7 C8 C9 -178.3(3) . . . . ?
C7 C8 C9 O5 0.9(5) . . . . ?
C7 C8 C9 O6 -178.9(3) . . . . ?
C8 N1 C4 C5 -1.3(5) . . . . ?
Re2 O12 C18 O11 179.9(2) . . . . ?
Re2 O12 C18 C17 -0.4(4) . . . . ?
Re2 N2 C13 C14 -177.9(2) . . . . ?
Re2 N2 C17 C16 178.5(3) . . . . ?
Re2 N2 C17 C18 0.3(3) . . . . ?
F2 C14 C15 C16 -178.5(3) . . . . ?
N2 C13 C14 F2 177.8(3) . . . . ?
N2 C13 C14 C15 -0.9(5) . . . . ?
N2 C17 C18 O11 179.7(3) . . . . ?
N2 C17 C18 O12 0.1(4) . . . . ?
C13 N2 C17 C16 -0.6(5) . . . . ?
C13 N2 C17 C18 -178.8(3) . . . . ?
C13 C14 C15 C16 0.1(6) . . . . ?
C14 C15 C16 C17 0.5(5) . . . . ?
C15 C16 C17 N2 -0.2(5) . . . . ?
C15 C16 C17 C18 177.8(3) . . . . ?
C16 C17 C18 O11 1.5(5) . . . . ?
C16 C17 C18 O12 -178.2(3) . . . . ?
C17 N2 C13 C14 1.1(5) . . . . ?


####################################################################### 
# 
# 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_35
_database_code_depnum_ccdc_archive 'CCDC 2205527'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-15
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H8 N O6 Re, H2 O'
_chemical_formula_sum            'C10 H10 N O7 Re'
_chemical_formula_weight         442.39
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   9.18810(10)
_cell_length_b                   11.06790(10)
_cell_length_c                   25.0097(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.9890(10)
_cell_angle_gamma                90
_cell_volume                     2518.63(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12874
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      79.1620
_cell_measurement_theta_min      3.5700
_shelx_estimated_absorpt_T_max   0.250
_shelx_estimated_absorpt_T_min   0.086
_exptl_absorpt_coefficient_mu    19.187
_exptl_absorpt_correction_T_max  0.308
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0561
0 0 -1 0.0561
-1 -1 0 0.0904
1 1 0 0.0904
0 -1 0 0.0502
0 1 0 0.0502
1 0 0 0.1186
-1 0 0 0.1186
2 0 -5 0.0978
0 1 1 0.0464
0 -1 1 0.0504
-4 5 1 0.0950
4 -5 -1 0.0950

_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10

_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13080
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         3.569
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    102.00 178.00   0.50    0.20    --  110.00 111.00  90.00  152
  2  ω     96.00 178.00   0.50    0.20    --  110.00  30.00 -30.00  164
  3  ω     96.00 178.00   0.50    0.20    --  110.00  30.00 -60.00  164
  4  ω    106.00 178.00   0.50    0.20    --  110.00  98.00-128.00  144
  5  ω     34.00 123.00   0.50    0.10    --   49.87  57.00 -60.00  178
  6  ω    -81.00 -11.00   0.50    0.20    --  -88.50  98.00-128.00  140
  7  ω   -125.00 -73.00   0.50    0.10    --  -49.87-125.00 -90.00  104
  8  ω   -165.00 -85.00   0.50    0.20    --  -88.50 -98.00 124.00  160
  9  ω   -125.00 -73.00   0.50    0.10    --  -49.87-125.00-150.00  104
 10  ω    -80.00  28.00   0.50    0.10    --  -49.87  98.00-128.00  216
 11  ω     36.00 134.00   0.50    0.20    --  110.00 -77.00 -60.00  196
 12  ω     34.00 124.00   0.50    0.20    --  110.00 -45.00 -30.00  180
 13  ω     34.00 108.00   0.50    0.20    --  110.00-111.00 -60.00  148
 14  ω     34.00 107.00   0.50    0.20    --  110.00 -94.00 -60.00  146
 15  ω     34.00 108.00   0.50    0.20    --  110.00-111.00-150.00  148
 16  ω     34.00 107.00   0.50    0.20    --  110.00 -94.00-180.00  146
 17  ω     34.00 107.00   0.50    0.20    --  110.00 -94.00-120.00  146
 18  ω     -6.00  84.00   0.50    0.10    --   49.87 -98.00 124.00  180
 19  ω     34.00 107.00   0.50    0.20    --  110.00 -98.00 124.00  146
 20  ω     38.00 127.00   0.50    0.20    --  110.00 -61.00  60.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0336750000
_diffrn_orient_matrix_UB_12      0.1310141000
_diffrn_orient_matrix_UB_13      -0.0185632000
_diffrn_orient_matrix_UB_21      -0.1460051000
_diffrn_orient_matrix_UB_22      -0.0049186000
_diffrn_orient_matrix_UB_23      0.0236743000
_diffrn_orient_matrix_UB_31      0.0788937000
_diffrn_orient_matrix_UB_32      0.0467339000
_diffrn_orient_matrix_UB_33      0.0544338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2557
_reflns_number_total             2565

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.452
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.000159(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0268P)²+10.9719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0575
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O7-H7B \\sim O7-H7C
 with sigma of 0.005
3. Others
 Fixed Sof: H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.38657(2) 0.81880(2) 0.63515(2) 0.02115(9) Uani 1 1 d . . . . .
O1 O 0.3891(4) 1.0947(3) 0.62927(14) 0.0482(9) Uani 1 1 d . . . . .
O2 O 0.6377(4) 0.8547(3) 0.72765(14) 0.0487(9) Uani 1 1 d . . . . .
O3 O 0.1719(4) 0.8468(4) 0.71679(15) 0.0500(9) Uani 1 1 d . . . . .
O4 O 0.5257(3) 0.7916(3) 0.57204(11) 0.0263(5) Uani 1 1 d . . . . .
O5 O 0.0793(3) 0.6641(2) 0.51527(11) 0.0260(6) Uani 1 1 d . . . . .
O6 O 0.2150(3) 0.7938(2) 0.56876(11) 0.0245(5) Uani 1 1 d . . . . .
N1 N 0.3652(3) 0.6187(3) 0.62495(12) 0.0198(6) Uani 1 1 d . . . . .
C1 C 0.3891(5) 0.9918(4) 0.63106(16) 0.0343(10) Uani 1 1 d . . . . .
C2 C 0.5457(5) 0.8385(4) 0.69269(17) 0.0324(9) Uani 1 1 d . . . . .
H4A H 0.497(6) 0.757(6) 0.545(3) 0.049 Uiso 1 1 d . U . . .
H4B H 0.563(7) 0.852(6) 0.559(3) 0.049 Uiso 1 1 d . U . . .
H7A H 0.153(6) 0.940(6) 0.541(2) 0.049 Uiso 1 1 d . U . . .
H7B H 0.219(9) 1.028(10) 0.515(4) 0.049 Uiso 0.5 1 d D U P A 1
C3 C 0.2543(5) 0.8351(4) 0.68655(17) 0.0317(9) Uani 1 1 d . . . . .
C4 C 0.4442(4) 0.5297(3) 0.65253(14) 0.0220(7) Uani 1 1 d . . . . .
C5 C 0.4187(4) 0.4086(4) 0.63833(15) 0.0269(8) Uani 1 1 d . . . . .
H5 H 0.476280 0.347384 0.657674 0.032 Uiso 1 1 calc R U . . .
C6 C 0.3112(4) 0.3769(3) 0.59671(18) 0.0302(8) Uani 1 1 d . . . . .
H6 H 0.294176 0.294500 0.587109 0.036 Uiso 1 1 calc R U . . .
C7 C 0.2282(4) 0.4682(3) 0.56906(15) 0.0255(7) Uani 1 1 d . . . . .
H7 H 0.152328 0.449729 0.540419 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2588(4) 0.5858(3) 0.58421(14) 0.0214(7) Uani 1 1 d . . . . .
C9 C 0.1761(4) 0.6872(3) 0.55326(14) 0.0212(7) Uani 1 1 d . . . . .
C10 C 0.5625(4) 0.5621(4) 0.69765(16) 0.0290(8) Uani 1 1 d . . . . .
H10A H 0.636392 0.612534 0.683656 0.044 Uiso 1 1 calc R U . . .
H10B H 0.609105 0.488207 0.713387 0.044 Uiso 1 1 calc R U . . .
H10C H 0.519524 0.606831 0.725442 0.044 Uiso 1 1 calc R U . . .
O7 O 0.1336(3) 1.0127(3) 0.52944(12) 0.0308(6) Uani 1 1 d D . . . .
H7C H 0.061(9) 0.993(11) 0.502(4) 0.046 Uiso 0.5 1 d D U P B 2


_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 O4 2.185(3) . ?
Re1 O6 2.142(3) . ?
Re1 N1 2.234(3) . ?
Re1 C1 1.918(5) . ?
Re1 C2 1.916(4) . ?
Re1 C3 1.896(5) . ?
O1 C1 1.139(6) . ?
O2 C2 1.143(5) . ?
O3 C3 1.149(6) . ?
O4 H4A 0.80(7) . ?
O4 H4B 0.83(7) . ?
O5 C9 1.234(5) . ?
O6 C9 1.278(4) . ?
N1 C4 1.354(5) . ?
N1 C8 1.360(5) . ?
C4 C5 1.398(5) . ?
C4 C10 1.498(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.373(5) . ?
C8 C9 1.508(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O7 H7A 0.87(7) . ?
O7 H7B 0.92(7) . ?
O7 H7C 0.92(7) . ?

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
O4 Re1 N1 80.33(11) . . ?
O6 Re1 O4 82.17(11) . . ?
O6 Re1 N1 74.95(10) . . ?
C1 Re1 O4 94.96(15) . . ?
C1 Re1 O6 95.76(13) . . ?
C1 Re1 N1 170.01(14) . . ?
C2 Re1 O4 95.53(16) . . ?
C2 Re1 O6 177.62(15) . . ?
C2 Re1 N1 104.15(14) . . ?
C2 Re1 C1 84.99(17) . . ?
C3 Re1 O4 175.49(15) . . ?
C3 Re1 O6 93.77(15) . . ?
C3 Re1 N1 96.75(15) . . ?
C3 Re1 C1 87.39(18) . . ?
C3 Re1 C2 88.51(19) . . ?
Re1 O4 H4A 122(4) . . ?
Re1 O4 H4B 119(4) . . ?
H4A O4 H4B 99(6) . . ?
C9 O6 Re1 119.9(2) . . ?
C4 N1 Re1 129.1(2) . . ?
C4 N1 C8 117.7(3) . . ?
C8 N1 Re1 113.2(2) . . ?
O1 C1 Re1 178.9(4) . . ?
O2 C2 Re1 177.0(4) . . ?
O3 C3 Re1 178.3(4) . . ?
N1 C4 C5 120.6(3) . . ?
N1 C4 C10 119.4(3) . . ?
C5 C4 C10 120.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 120.8 . . ?
C5 C6 C7 118.4(4) . . ?
C7 C6 H6 120.8 . . ?
C6 C7 H7 120.8 . . ?
C8 C7 C6 118.3(4) . . ?
C8 C7 H7 120.8 . . ?
N1 C8 C7 124.0(3) . . ?
N1 C8 C9 116.3(3) . . ?
C7 C8 C9 119.7(3) . . ?
O5 C9 O6 124.5(3) . . ?
O5 C9 C8 119.9(3) . . ?
O6 C9 C8 115.6(3) . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H7A O7 H7B 98(8) . . ?
H7A O7 H7C 97(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
O4 H4A O5 0.80(7) 1.87(7) 2.665(4) 174(6) 2_556 yes
O4 H4B O7 0.83(7) 1.83(7) 2.665(4) 176(6) 6_675 yes
O7 H7A O6 0.87(7) 1.82(7) 2.682(4) 173(6) . yes
O7 H7B O7 0.92(7) 1.88(8) 2.760(6) 160(10) 2_556 yes
C6 H6 O1 0.95 2.55 3.282(5) 133.8 1_545 yes

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
Re1 O6 C9 O5 -179.5(3) . . . . ?
Re1 O6 C9 C8 -0.4(4) . . . . ?
Re1 N1 C4 C5 -176.9(3) . . . . ?
Re1 N1 C4 C10 1.5(5) . . . . ?
Re1 N1 C8 C7 177.8(3) . . . . ?
Re1 N1 C8 C9 0.5(4) . . . . ?
N1 C4 C5 C6 -1.1(6) . . . . ?
N1 C8 C9 O5 179.0(3) . . . . ?
N1 C8 C9 O6 -0.1(5) . . . . ?
C4 N1 C8 C7 -0.8(5) . . . . ?
C4 N1 C8 C9 -178.2(3) . . . . ?
C4 C5 C6 C7 -0.1(6) . . . . ?
C5 C6 C7 C8 0.8(6) . . . . ?
C6 C7 C8 N1 -0.3(6) . . . . ?
C6 C7 C8 C9 176.9(3) . . . . ?
C7 C8 C9 O5 1.5(5) . . . . ?
C7 C8 C9 O6 -177.6(3) . . . . ?
C8 N1 C4 C5 1.6(5) . . . . ?
C8 N1 C4 C10 179.9(3) . . . . ?
C10 C4 C5 C6 -179.5(4) . . . . ?


####################################################################### 
# 
# 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_41
_database_code_depnum_ccdc_archive 'CCDC 2205529'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(C9 H5 N2 O8 Re), H2 O'
_chemical_formula_sum            'C27 H17 N6 O25 Re3'
_chemical_formula_weight         1384.06
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.13580(10)
_cell_length_b                   18.60120(10)
_cell_length_c                   16.12660(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.2970(10)
_cell_angle_gamma                90
_cell_volume                     3640.38(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    49870
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.5590
_cell_measurement_theta_min      2.3540
_shelx_estimated_absorpt_T_max   0.379
_shelx_estimated_absorpt_T_min   0.068
_exptl_absorpt_coefficient_mu    20.072
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2584
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.0306
1 0 -1 0.0306
0 1 0 0.0503
0 -1 0 0.0463
5 1 4 0.1132
-4 2 -5 0.1371
-1 -7 8 0.0831
-1 -1 1 0.0249
-4 5 4 0.0392
4 -5 1 0.0800

_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06

_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71970
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.627
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.00    --  -41.94 125.00-180.00   81
  2  ω   -116.00 -18.00   1.00    1.00    --  -41.94 -37.00 -90.00   98
  3  ω    -70.00  31.00   1.00    1.00    --  -41.94  57.00-180.00  101
  4  ω    -66.00  33.00   1.00    1.00    --  -41.94  37.00  90.00   99
  5  ω      8.00  34.00   1.00    1.00    --   41.94  83.00 -11.78   26
  6  ω      8.00  42.00   1.00    1.00    --   41.94  82.00  65.40   34
  7  ω     36.00 109.00   1.00    2.00    --  112.00-111.00 120.00   73
  8  ω     29.00 107.00   1.00    2.00    --  112.00 -94.00  30.00   78
  9  ω     36.00 109.00   1.00    2.00    --  112.00-111.00 -60.00   73
 10  ω     36.00 109.00   1.00    2.00    --  112.00-111.00-150.00   73
 11  ω     36.00 109.00   1.00    2.00    --  112.00-111.00-180.00   73
 12  ω     36.00 109.00   1.00    2.00    --  112.00-111.00 150.00   73
 13  ω    104.00 178.00   1.00    2.00    --  112.00 111.00   0.00   74
 14  ω     83.00 178.00   1.00    2.00    --  112.00  59.00 171.43   95
 15  ω    103.00 178.00   1.00    2.00    --  112.00  77.00-180.00   75
 16  ω     36.00 109.00   1.00    2.00    --  112.00-111.00 -30.00   73
 17  ω    104.00 178.00   1.00    2.00    --  112.00 111.00  90.00   74
 18  ω    103.00 178.00   1.00    2.00    --  112.00  77.00 -90.00   75
 19  ω     36.00 145.00   1.00    2.00    --  112.00 -77.00   0.00  109
 20  ω     36.00 109.00   1.00    2.00    --  112.00-111.00  90.00   73
 21  ω     29.00 107.00   1.00    2.00    --  112.00 -94.00   0.00   78
 22  ω     36.00 109.00   1.00    2.00    --  112.00-111.00-120.00   73
 23  ω     85.00 178.00   1.00    2.00    --  112.00  52.00-104.98   93
 24  ω     29.00 107.00   1.00    2.00    --  112.00 -94.00 -30.00   78
 25  ω    103.00 178.00   1.00    2.00    --  112.00  77.00-150.00   75
 26  ω     36.00 109.00   1.00    2.00    --  112.00-111.00 -90.00   73
 27  ω     82.00 178.00   1.00    2.00    --  112.00  66.00  45.97   96
 28  ω     84.00 178.00   1.00    2.00    --  112.00  30.00 150.00   94
 29  ω     36.00 109.00   1.00    2.00    --  112.00-111.00   0.00   73
 30  ω    104.00 178.00   1.00    2.00    --  112.00 111.00  60.00   74
 31  ω   -116.00 -18.00   1.00    1.00    --  -41.94 -37.00 120.00   98
 32  ω    -87.00  -6.00   1.00    1.00    --  -41.94 125.00 -90.00   81
 33  ω   -116.00 -18.00   1.00    1.00    --  -41.94 -37.00  30.00   98
 34  ω      8.00  42.00   1.00    1.00    --   41.94  82.00-145.98   34
 35  ω      8.00  42.00   1.00    1.00    --   41.94  81.00 -92.55   34
 36  ω      8.00  34.00   1.00    1.00    --   41.94  83.00  40.59   26
 37  ω      9.00  42.00   1.00    1.00    --   41.94  79.00 155.05   33
 38  ω     83.00 137.00   1.00    2.00    --  112.00  59.00  26.75   54
 39  ω     82.00 178.00   1.00    2.00    --  112.00  65.00 -72.21   96
 40  ω     81.00 178.00   1.00    2.00    --  112.00  69.00-156.10   97
 41  ω     83.00 178.00   1.00    2.00    --  112.00  61.00   0.00   95
 42  ω     85.00 178.00   1.00    2.00    --  112.00  53.00  86.88   93
 43  ω     85.00 178.00   1.00    2.00    --  112.00  49.00 -20.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1231517000
_diffrn_orient_matrix_UB_12      0.0169292000
_diffrn_orient_matrix_UB_13      0.0120794000
_diffrn_orient_matrix_UB_21      0.0286393000
_diffrn_orient_matrix_UB_22      0.0458629000
_diffrn_orient_matrix_UB_23      0.0767005000
_diffrn_orient_matrix_UB_31      0.0115538000
_diffrn_orient_matrix_UB_32      0.0668096000
_diffrn_orient_matrix_UB_33      -0.0556954000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7403
_reflns_number_total             7431

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.746
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.000244(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.263
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0171P)²+5.1003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0446
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O22A-N6 \\sim O22B-N6 \\sim O21B-N6 \\sim O21A-N6
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
O21A \\sim O21B \\sim O22A \\sim O22B: within 3A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 3A
4. Others
 Sof(O21B)=Sof(O22B)=1-FVAR(1)
 Sof(O21A)=Sof(O22A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.5767(3) 0.48638(17) 0.79113(19) 0.0288(6) Uani 1 1 d . . . . .
C2 C 0.5730(2) 0.60539(15) 0.70342(17) 0.0211(5) Uani 1 1 d . . . . .
C3 C 0.7511(3) 0.57302(16) 0.79339(19) 0.0259(6) Uani 1 1 d . . . . .
C4 C 0.6312(2) 0.75794(15) 0.83523(17) 0.0200(5) Uani 1 1 d . . . . .
C5 C 0.6406(3) 0.82362(16) 0.87421(19) 0.0257(6) Uani 1 1 d . . . . .
H5 H 0.646213 0.867153 0.843708 0.031 Uiso 1 1 calc R U . . .
C6 C 0.6415(3) 0.82295(18) 0.9599(2) 0.0302(7) Uani 1 1 d . . . . .
H6 H 0.647079 0.866690 0.990042 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6342(3) 0.75809(18) 1.00145(19) 0.0277(6) Uani 1 1 d . . . . .
H7 H 0.635754 0.756720 1.060327 0.033 Uiso 1 1 calc R U . . .
C8 C 0.6245(2) 0.69515(16) 0.95605(17) 0.0215(5) Uani 1 1 d . . . . .
C9 C 0.6185(2) 0.62281(17) 0.99780(18) 0.0249(6) Uani 1 1 d . . . . .
N1 N 0.62254(19) 0.69432(12) 0.87196(14) 0.0181(4) Uani 1 1 d . . . . .
N2 N 0.6317(2) 0.75664(12) 0.74401(15) 0.0220(5) Uani 1 1 d . . . . .
O1 O 0.5651(3) 0.42614(13) 0.77588(18) 0.0462(7) Uani 1 1 d . . . . .
O2 O 0.5547(2) 0.61685(12) 0.63465(13) 0.0297(5) Uani 1 1 d . . . . .
O3 O 0.8426(2) 0.56583(14) 0.77781(16) 0.0362(5) Uani 1 1 d . . . . .
O4 O 0.42862(17) 0.60768(12) 0.85155(14) 0.0231(4) Uani 1 1 d . . . . .
H4A H 0.385(3) 0.590(2) 0.816(3) 0.031(10) Uiso 1 1 d . . . . .
H4B H 0.413(4) 0.590(2) 0.894(3) 0.037(12) Uiso 1 1 d . . . . .
O5 O 0.7176(2) 0.74060(14) 0.71038(14) 0.0365(5) Uani 1 1 d . . . . .
O6 O 0.5463(2) 0.77231(15) 0.70925(15) 0.0397(6) Uani 1 1 d . . . . .
O7 O 0.6232(2) 0.61896(14) 1.07353(13) 0.0330(5) Uani 1 1 d . . . . .
O8 O 0.60857(18) 0.56900(11) 0.94833(13) 0.0261(4) Uani 1 1 d . . . . .
Re1 Re 0.59879(2) 0.58533(2) 0.81777(2) 0.01826(4) Uani 1 1 d . . . . .
C10 C 0.2090(3) 0.46516(17) 0.43458(18) 0.0260(6) Uani 1 1 d . . . . .
C11 C 0.2135(2) 0.59549(17) 0.37603(19) 0.0249(6) Uani 1 1 d . . . . .
C12 C 0.3967(2) 0.54518(15) 0.43951(18) 0.0224(6) Uani 1 1 d . . . . .
C13 C 0.3024(2) 0.72169(16) 0.53252(19) 0.0237(6) Uani 1 1 d . . . . .
C14 C 0.3130(3) 0.77938(17) 0.5854(2) 0.0330(7) Uani 1 1 d . . . . .
H14 H 0.323212 0.826777 0.564895 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3084(3) 0.76569(17) 0.6694(2) 0.0343(7) Uani 1 1 d . . . . .
H15 H 0.313334 0.803917 0.708307 0.041 Uiso 1 1 calc R U . . .
C16 C 0.2964(3) 0.69531(17) 0.6962(2) 0.0284(6) Uani 1 1 d . . . . .
H16 H 0.292540 0.684617 0.753700 0.034 Uiso 1 1 calc R U . . .
C17 C 0.2903(2) 0.64109(15) 0.63810(18) 0.0214(5) Uani 1 1 d . . . . .
C18 C 0.2881(2) 0.56258(15) 0.66263(18) 0.0199(5) Uani 1 1 d . . . . .
N3 N 0.29035(19) 0.65335(12) 0.55527(15) 0.0196(5) Uani 1 1 d . . . . .
N4 N 0.3064(2) 0.73574(14) 0.44228(17) 0.0289(6) Uani 1 1 d . . . . .
O9 O 0.1824(2) 0.41109(13) 0.40680(16) 0.0378(6) Uani 1 1 d . . . . .
O10 O 0.1908(2) 0.61808(14) 0.31159(14) 0.0359(5) Uani 1 1 d . . . . .
O11 O 0.48369(18) 0.54036(13) 0.41366(15) 0.0319(5) Uani 1 1 d . . . . .
O12 O 0.3839(2) 0.71184(14) 0.40384(16) 0.0400(6) Uani 1 1 d . . . . .
O13 O 0.2325(2) 0.77207(17) 0.41334(18) 0.0524(8) Uani 1 1 d . . . . .
O14 O 0.29836(18) 0.54709(12) 0.73720(13) 0.0263(4) Uani 1 1 d . . . . .
O15 O 0.27886(16) 0.51766(10) 0.60454(12) 0.0206(4) Uani 1 1 d . . . . .
O16 O 0.08939(18) 0.57210(13) 0.54135(14) 0.0240(4) Uani 1 1 d . . . . .
H16A H 0.044(4) 0.582(2) 0.503(3) 0.045(13) Uiso 1 1 d . . . . .
H16B H 0.074(5) 0.535(3) 0.563(4) 0.08(2) Uiso 1 1 d . . . . .
Re2 Re 0.25059(2) 0.55615(2) 0.48144(2) 0.01768(4) Uani 1 1 d . . . . .
C20 C 0.1040(3) 0.52847(16) 0.88783(19) 0.0262(6) Uani 1 1 d . . . . .
C21 C -0.0692(3) 0.43916(16) 0.87892(19) 0.0253(6) Uani 1 1 d . . . . .
C22 C 0.1137(2) 0.40189(15) 0.95658(18) 0.0220(6) Uani 1 1 d . . . . .
C23 C 0.0367(2) 0.26593(16) 0.80318(19) 0.0228(6) Uani 1 1 d . . . . .
C24 C 0.0223(3) 0.20631(18) 0.7538(2) 0.0336(7) Uani 1 1 d . . . . .
H24 H 0.009499 0.160049 0.776786 0.040 Uiso 1 1 calc R U . . .
C25 C 0.0274(3) 0.2171(2) 0.6690(2) 0.0389(8) Uani 1 1 d . . . . .
H25 H 0.020237 0.177656 0.631983 0.047 Uiso 1 1 calc R U . . .
C26 C 0.0429(3) 0.28559(19) 0.6386(2) 0.0314(7) Uani 1 1 d . . . . .
H26 H 0.046617 0.293785 0.580510 0.038 Uiso 1 1 calc R U . . .
C27 C 0.0530(2) 0.34208(16) 0.69353(18) 0.0225(6) Uani 1 1 d . . . . .
C28 C 0.0575(2) 0.41952(17) 0.66500(18) 0.0231(6) Uani 1 1 d . . . . .
N5 N 0.05307(19) 0.33255(13) 0.77695(14) 0.0195(5) Uani 1 1 d . . . . .
N6 N 0.03287(18) 0.25501(13) 0.89405(17) 0.0276(5) Uani 1 1 d D . . . .
O17 O 0.1171(2) 0.58568(13) 0.91235(17) 0.0406(6) Uani 1 1 d . . . . .
O18 O -0.1593(2) 0.44076(14) 0.89907(16) 0.0382(6) Uani 1 1 d . . . . .
O19 O 0.1339(2) 0.38512(14) 1.02352(13) 0.0336(5) Uani 1 1 d . . . . .
O20 O 0.24884(17) 0.41863(12) 0.79888(13) 0.0205(4) Uani 1 1 d . . . . .
H20A H 0.290(4) 0.408(2) 0.837(3) 0.042(12) Uiso 1 1 d . . . . .
H20B H 0.265(3) 0.454(2) 0.776(3) 0.031(11) Uiso 1 1 d . . . . .
O21A O 0.1125(6) 0.2351(6) 0.9334(6) 0.0484(19) Uani 0.584(17) 1 d D U P A 1
O21B O 0.1242(6) 0.2574(7) 0.9257(8) 0.038(2) Uani 0.416(17) 1 d D U P A 2
O22A O -0.0554(4) 0.2718(6) 0.9259(4) 0.0494(18) Uani 0.584(17) 1 d D U P A 1
O22B O -0.0511(6) 0.2338(8) 0.9263(5) 0.048(2) Uani 0.416(17) 1 d D U P A 2
O23 O 0.05325(18) 0.43275(13) 0.58936(13) 0.0298(5) Uani 1 1 d . . . . .
O24 O 0.06312(17) 0.46660(11) 0.72112(12) 0.0235(4) Uani 1 1 d . . . . .
Re3 Re 0.08119(2) 0.43346(2) 0.84649(2) 0.01635(4) Uani 1 1 d . . . . .
O25 O 0.3528(2) 0.56520(13) 0.99336(15) 0.0325(5) Uani 1 1 d . . . . .
H25A H 0.375(3) 0.523(2) 1.009(3) 0.039 Uiso 1 1 d . U . . .
H25B H 0.286(4) 0.566(2) 1.004(3) 0.039 Uiso 1 1 d . 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
C1 O1 1.156(4) . ?
C1 Re1 1.909(3) . ?
C2 O2 1.150(4) . ?
C2 Re1 1.906(3) . ?
C3 O3 1.147(4) . ?
C3 Re1 1.906(3) . ?
C4 C5 1.379(4) . ?
C4 N1 1.328(4) . ?
C4 N2 1.471(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(4) . ?
C8 C9 1.507(4) . ?
C8 N1 1.356(4) . ?
C9 O7 1.224(4) . ?
C9 O8 1.285(4) . ?
N1 Re1 2.226(2) . ?
N2 O5 1.215(3) . ?
N2 O6 1.211(3) . ?
O4 H4A 0.84(4) . ?
O4 H4B 0.79(5) . ?
O4 Re1 2.179(2) . ?
O8 Re1 2.130(2) . ?
C10 O9 1.147(4) . ?
C10 Re2 1.920(3) . ?
C11 O10 1.153(4) . ?
C11 Re2 1.903(3) . ?
C12 O11 1.140(4) . ?
C12 Re2 1.912(3) . ?
C13 C14 1.377(5) . ?
C13 N3 1.331(4) . ?
C13 N4 1.480(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.386(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.378(4) . ?
C17 C18 1.513(4) . ?
C17 N3 1.355(4) . ?
C18 O14 1.242(4) . ?
C18 O15 1.260(4) . ?
N3 Re2 2.217(2) . ?
N4 O12 1.213(4) . ?
N4 O13 1.214(4) . ?
O15 Re2 2.1364(19) . ?
O16 H16A 0.84(5) . ?
O16 H16B 0.79(6) . ?
O16 Re2 2.206(2) . ?
C20 O17 1.146(4) . ?
C20 Re3 1.908(3) . ?
C21 O18 1.144(4) . ?
C21 Re3 1.904(3) . ?
C22 O19 1.149(4) . ?
C22 Re3 1.909(3) . ?
C23 C24 1.376(4) . ?
C23 N5 1.325(4) . ?
C23 N6 1.480(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.385(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.377(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(4) . ?
C27 C28 1.513(4) . ?
C27 N5 1.357(4) . ?
C28 O23 1.245(4) . ?
C28 O24 1.261(4) . ?
N5 Re3 2.212(2) . ?
N6 O21A 1.212(4) . ?
N6 O21B 1.219(4) . ?
N6 O22A 1.230(4) . ?
N6 O22B 1.212(4) . ?
O20 H20A 0.81(5) . ?
O20 H20B 0.78(4) . ?
O20 Re3 2.196(2) . ?
O24 Re3 2.1240(19) . ?
O25 H25A 0.87(5) . ?
O25 H25B 0.83(5) . ?

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
O1 C1 Re1 178.7(3) . . ?
O2 C2 Re1 178.3(3) . . ?
O3 C3 Re1 179.2(3) . . ?
C5 C4 N2 118.0(3) . . ?
N1 C4 C5 126.4(3) . . ?
N1 C4 N2 115.6(2) . . ?
C4 C5 H5 121.7 . . ?
C4 C5 C6 116.6(3) . . ?
C6 C5 H5 121.7 . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C7 119.5(3) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.1(3) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 121.5(3) . . ?
N1 C8 C7 122.6(3) . . ?
N1 C8 C9 115.9(3) . . ?
O7 C9 C8 119.7(3) . . ?
O7 C9 O8 125.3(3) . . ?
O8 C9 C8 115.0(2) . . ?
C4 N1 C8 115.8(2) . . ?
C4 N1 Re1 130.32(19) . . ?
C8 N1 Re1 113.86(18) . . ?
O5 N2 C4 117.3(2) . . ?
O6 N2 C4 116.8(2) . . ?
O6 N2 O5 125.9(3) . . ?
H4A O4 H4B 106(4) . . ?
Re1 O4 H4A 110(3) . . ?
Re1 O4 H4B 112(3) . . ?
C9 O8 Re1 120.47(19) . . ?
C1 Re1 N1 169.89(11) . . ?
C1 Re1 O4 96.20(12) . . ?
C1 Re1 O8 95.28(11) . . ?
C2 Re1 C1 87.07(13) . . ?
C2 Re1 N1 102.81(10) . . ?
C2 Re1 O4 93.05(11) . . ?
C2 Re1 O8 172.95(10) . . ?
C3 Re1 C1 88.45(14) . . ?
C3 Re1 C2 88.78(13) . . ?
C3 Re1 N1 93.82(11) . . ?
C3 Re1 O4 175.08(11) . . ?
C3 Re1 O8 97.92(11) . . ?
O4 Re1 N1 81.32(8) . . ?
O8 Re1 N1 74.65(8) . . ?
O8 Re1 O4 80.10(9) . . ?
O9 C10 Re2 178.9(3) . . ?
O10 C11 Re2 178.8(3) . . ?
O11 C12 Re2 178.2(3) . . ?
C14 C13 N4 117.9(3) . . ?
N3 C13 C14 125.7(3) . . ?
N3 C13 N4 116.3(3) . . ?
C13 C14 H14 121.3 . . ?
C13 C14 C15 117.4(3) . . ?
C15 C14 H14 121.3 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.0(3) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 C18 122.0(3) . . ?
N3 C17 C16 123.1(3) . . ?
N3 C17 C18 114.8(2) . . ?
O14 C18 C17 118.4(3) . . ?
O14 C18 O15 125.0(3) . . ?
O15 C18 C17 116.6(2) . . ?
C13 N3 C17 115.7(3) . . ?
C13 N3 Re2 130.9(2) . . ?
C17 N3 Re2 113.01(18) . . ?
O12 N4 C13 117.9(3) . . ?
O12 N4 O13 125.5(3) . . ?
O13 N4 C13 116.6(3) . . ?
C18 O15 Re2 118.82(18) . . ?
H16A O16 H16B 110(5) . . ?
Re2 O16 H16A 107(3) . . ?
Re2 O16 H16B 107(4) . . ?
C10 Re2 N3 170.56(11) . . ?
C10 Re2 O15 96.37(10) . . ?
C10 Re2 O16 93.39(11) . . ?
C11 Re2 C10 85.81(13) . . ?
C11 Re2 C12 86.61(12) . . ?
C11 Re2 N3 102.48(11) . . ?
C11 Re2 O15 174.39(10) . . ?
C11 Re2 O16 97.65(11) . . ?
C12 Re2 C10 90.53(13) . . ?
C12 Re2 N3 94.43(11) . . ?
C12 Re2 O15 98.51(10) . . ?
C12 Re2 O16 174.41(11) . . ?
O15 Re2 N3 74.97(8) . . ?
O15 Re2 O16 77.09(8) . . ?
O16 Re2 N3 81.15(8) . . ?
O17 C20 Re3 179.6(3) . . ?
O18 C21 Re3 178.2(3) . . ?
O19 C22 Re3 177.8(3) . . ?
C24 C23 N6 117.2(3) . . ?
N5 C23 C24 126.0(3) . . ?
N5 C23 N6 116.7(3) . . ?
C23 C24 H24 121.7 . . ?
C23 C24 C25 116.6(3) . . ?
C25 C24 H24 121.7 . . ?
C24 C25 H25 120.2 . . ?
C26 C25 C24 119.5(3) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 120.4 . . ?
C25 C26 C27 119.2(3) . . ?
C27 C26 H26 120.4 . . ?
C26 C27 C28 122.2(3) . . ?
N5 C27 C26 122.5(3) . . ?
N5 C27 C28 115.2(3) . . ?
O23 C28 C27 119.0(3) . . ?
O23 C28 O24 124.6(3) . . ?
O24 C28 C27 116.4(2) . . ?
C23 N5 C27 116.1(3) . . ?
C23 N5 Re3 130.9(2) . . ?
C27 N5 Re3 113.01(19) . . ?
O21A N6 C23 122.1(6) . . ?
O21A N6 O22A 123.5(6) . . ?
O21B N6 C23 112.1(7) . . ?
O22A N6 C23 114.2(4) . . ?
O22B N6 C23 120.0(5) . . ?
O22B N6 O21B 126.6(7) . . ?
H20A O20 H20B 114(4) . . ?
Re3 O20 H20A 109(3) . . ?
Re3 O20 H20B 107(3) . . ?
C28 O24 Re3 119.11(19) . . ?
C20 Re3 C22 86.05(13) . . ?
C20 Re3 N5 169.91(11) . . ?
C20 Re3 O20 96.07(11) . . ?
C20 Re3 O24 94.46(11) . . ?
C21 Re3 C20 89.41(13) . . ?
C21 Re3 C22 87.44(12) . . ?
C21 Re3 N5 92.35(11) . . ?
C21 Re3 O20 173.86(11) . . ?
C21 Re3 O24 98.68(11) . . ?
C22 Re3 N5 103.95(11) . . ?
C22 Re3 O20 95.69(10) . . ?
C22 Re3 O24 173.86(10) . . ?
O20 Re3 N5 81.78(8) . . ?
O24 Re3 N5 75.45(8) . . ?
O24 Re3 O20 78.17(8) . . ?
H25A O25 H25B 105(4) . . ?

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
O4 H4A O14 0.84(4) 1.83(4) 2.672(3) 176(4) . yes
O4 H4B O25 0.79(5) 1.82(5) 2.593(3) 167(4) . yes
O16 H16A O23 0.84(5) 1.92(5) 2.722(3) 159(4) 3_566 yes
O16 H16B O23 0.79(6) 1.97(6) 2.741(3) 165(6) . yes
O20 H20A O7 0.81(5) 1.86(5) 2.665(3) 177(5) 3_667 yes
O20 H20B O14 0.78(4) 1.89(5) 2.658(3) 170(4) . yes
O25 H25A O8 0.87(5) 1.86(5) 2.708(3) 167(4) 3_667 yes
O25 H25B O17 0.83(5) 2.54(4) 3.162(4) 132(4) . yes
O25 H25B O18 0.83(5) 2.20(5) 2.929(3) 146(4) 3_567 yes

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
C4 C5 C6 C7 0.6(5) . . . . ?
C5 C4 N1 C8 -0.8(4) . . . . ?
C5 C4 N1 Re1 176.7(2) . . . . ?
C5 C4 N2 O5 100.0(3) . . . . ?
C5 C4 N2 O6 -79.4(4) . . . . ?
C5 C6 C7 C8 -0.9(5) . . . . ?
C6 C7 C8 C9 178.8(3) . . . . ?
C6 C7 C8 N1 0.4(5) . . . . ?
C7 C8 C9 O7 -0.6(4) . . . . ?
C7 C8 C9 O8 179.3(3) . . . . ?
C7 C8 N1 C4 0.4(4) . . . . ?
C7 C8 N1 Re1 -177.4(2) . . . . ?
C8 C9 O8 Re1 -1.1(3) . . . . ?
C9 C8 N1 C4 -178.0(2) . . . . ?
C9 C8 N1 Re1 4.1(3) . . . . ?
N1 C4 C5 C6 0.2(5) . . . . ?
N1 C4 N2 O5 -79.4(3) . . . . ?
N1 C4 N2 O6 101.2(3) . . . . ?
N1 C8 C9 O7 177.9(3) . . . . ?
N1 C8 C9 O8 -2.2(4) . . . . ?
N2 C4 C5 C6 -179.1(3) . . . . ?
N2 C4 N1 C8 178.6(2) . . . . ?
N2 C4 N1 Re1 -4.0(4) . . . . ?
O7 C9 O8 Re1 178.9(2) . . . . ?
C13 C14 C15 C16 1.7(5) . . . . ?
C14 C13 N3 C17 -0.9(4) . . . . ?
C14 C13 N3 Re2 170.9(2) . . . . ?
C14 C13 N4 O12 113.6(3) . . . . ?
C14 C13 N4 O13 -64.6(4) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C15 C16 C17 C18 174.1(3) . . . . ?
C15 C16 C17 N3 -3.1(5) . . . . ?
C16 C17 C18 O14 -4.1(4) . . . . ?
C16 C17 C18 O15 177.8(3) . . . . ?
C16 C17 N3 C13 3.2(4) . . . . ?
C16 C17 N3 Re2 -170.0(2) . . . . ?
C17 C18 O15 Re2 -6.3(3) . . . . ?
C18 C17 N3 C13 -174.1(2) . . . . ?
C18 C17 N3 Re2 12.6(3) . . . . ?
N3 C13 C14 C15 -1.6(5) . . . . ?
N3 C13 N4 O12 -65.4(4) . . . . ?
N3 C13 N4 O13 116.4(3) . . . . ?
N3 C17 C18 O14 173.3(3) . . . . ?
N3 C17 C18 O15 -4.8(4) . . . . ?
N4 C13 C14 C15 179.6(3) . . . . ?
N4 C13 N3 C17 178.0(2) . . . . ?
N4 C13 N3 Re2 -10.2(4) . . . . ?
O14 C18 O15 Re2 175.7(2) . . . . ?
C23 C24 C25 C26 -1.9(5) . . . . ?
C24 C23 N5 C27 1.5(4) . . . . ?
C24 C23 N5 Re3 -178.5(2) . . . . ?
C24 C23 N6 O21A 83.3(7) . . . . ?
C24 C23 N6 O21B 104.9(8) . . . . ?
C24 C23 N6 O22A -100.7(6) . . . . ?
C24 C23 N6 O22B -63.2(9) . . . . ?
C24 C25 C26 C27 0.0(5) . . . . ?
C25 C26 C27 C28 -173.1(3) . . . . ?
C25 C26 C27 N5 2.9(5) . . . . ?
C26 C27 C28 O23 -0.9(4) . . . . ?
C26 C27 C28 O24 177.7(3) . . . . ?
C26 C27 N5 C23 -3.6(4) . . . . ?
C26 C27 N5 Re3 176.4(2) . . . . ?
C27 C28 O24 Re3 5.8(3) . . . . ?
C28 C27 N5 C23 172.7(2) . . . . ?
C28 C27 N5 Re3 -7.4(3) . . . . ?
N5 C23 C24 C25 1.2(5) . . . . ?
N5 C23 N6 O21A -97.2(7) . . . . ?
N5 C23 N6 O21B -75.5(8) . . . . ?
N5 C23 N6 O22A 78.9(6) . . . . ?
N5 C23 N6 O22B 116.4(9) . . . . ?
N5 C27 C28 O23 -177.1(3) . . . . ?
N5 C27 C28 O24 1.4(4) . . . . ?
N6 C23 C24 C25 -179.3(3) . . . . ?
N6 C23 N5 C27 -178.0(2) . . . . ?
N6 C23 N5 Re3 2.0(4) . . . . ?
O23 C28 O24 Re3 -175.7(2) . . . . ?


####################################################################### 
# 
# 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_26
_database_code_depnum_ccdc_archive 'CCDC 2205522'
loop_
_audit_author_name
_audit_author_address
'Olivier Blacque'
;Department of Chemistry, University of Zurich
Switzerland
;
_audit_update_record             
;
2022-09-06 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;

_audit_creation_date             2021-03-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C10 H5 N2 O6 Re), 3(H2 O)'
_chemical_formula_sum            'C20 H16 N4 O15 Re2'
_chemical_formula_weight         924.77
_chemical_melting_point          ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9380(3)
_cell_length_b                   11.4782(3)
_cell_length_c                   12.8234(3)
_cell_angle_alpha                101.726(2)
_cell_angle_beta                 111.100(3)
_cell_angle_gamma                109.637(3)
_cell_volume                     1314.84(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18113
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3200
_cell_measurement_theta_min      3.9420
_shelx_estimated_absorpt_T_max   0.459
_shelx_estimated_absorpt_T_min   0.062
_exptl_absorpt_coefficient_mu    18.475
_exptl_absorpt_correction_T_max  0.461
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0301
0 -1 0 0.0201
5 -2 0 0.0753
-5 2 0 0.0553
2 2 -5 0.1424
2 -3 5 0.0884

_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05

_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23312
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.976
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  27.00   0.80    1.00    --  -42.61  57.00-180.00  120
  2  ω    -74.00  30.00   0.80    1.00    --  -42.61  77.00 -60.00  130
  3  ω   -113.00 -17.00   0.80    1.00    --  -42.61 -57.00  30.00  120
  4  ω     10.00  42.00   0.80    1.00    --   42.61  81.00   4.31   40
  5  ω     11.00  40.60   0.80    1.00    --   42.61  77.00-145.88   37
  6  ω    -21.00  73.40   0.80    1.00    --   42.61 -77.00 -90.00  118
  7  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00-150.00   95
  8  ω     41.00 138.60   0.80    2.00    --  111.00 -61.00 -60.00  122
  9  ω     36.00 108.00   0.80    2.00    --  111.00-111.00 120.00   90
 10  ω    104.00 177.60   0.80    2.00    --  111.00 111.00-120.00   92
 11  ω    104.00 177.60   0.80    2.00    --  111.00 111.00   0.00   92
 12  ω     36.00 108.00   0.80    2.00    --  111.00-111.00 -30.00   90
 13  ω     87.00 177.40   0.80    2.00    --  111.00  30.00-120.00  113
 14  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00 -90.00   95
 15  ω     36.00 108.00   0.80    2.00    --  111.00-111.00-150.00   90
 16  ω     36.00 134.40   0.80    2.00    --  111.00 -30.00 -90.00  123
 17  ω     36.00 108.00   0.80    2.00    --  111.00-111.00  30.00   90
 18  ω     36.00 108.00   0.80    2.00    --  111.00-111.00  90.00   90
 19  ω    104.00 177.60   0.80    2.00    --  111.00 111.00 -90.00   92
 20  ω     36.00 134.40   0.80    2.00    --  111.00 -30.00-180.00  123
 21  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00 150.00   95
 22  ω    103.00 177.40   0.80    2.00    --  111.00  77.00 120.00   93
 23  ω     87.00 177.40   0.80    2.00    --  111.00  45.00 -90.00  113
 24  ω     37.00 141.00   0.80    2.00    --  111.00 -77.00 -90.00  130
 25  ω    103.00 177.40   0.80    2.00    --  111.00  77.00  30.00   93
 26  ω     30.00 106.00   0.80    2.00    --  111.00 -94.00-120.00   95
 27  ω    104.00 177.60   0.80    2.00    --  111.00 111.00-150.00   92
 28  ω     87.00 177.40   0.80    2.00    --  111.00  30.00-180.00  113
 29  ω   -116.00 -20.00   0.80    1.00    --  -42.61 -37.00 -90.00  120
 30  ω   -113.00 -17.00   0.80    1.00    --  -42.61 -57.00 120.00  120
 31  ω    -65.00  29.40   0.80    1.00    --  -42.61  37.00  90.00  118
 32  ω     10.00  42.00   0.80    1.00    --   42.61  80.00  54.70   40
 33  ω     11.00  40.60   0.80    1.00    --   42.61  79.00-109.67   37
 34  ω     10.00  42.00   0.80    1.00    --   42.61  81.00 156.05   40
 35  ω     11.00  40.60   0.80    1.00    --   42.61  78.00 -67.33   37
 36  ω     83.00 177.40   0.80    2.00    --  111.00  64.00-172.63  118
 37  ω     83.00 177.40   0.80    2.00    --  111.00  61.00 120.00  118
 38  ω     83.00 177.40   0.80    2.00    --  111.00  61.00  30.00  118
 39  ω     83.00 177.40   0.80    2.00    --  111.00  61.00 -60.00  118
 40  ω     83.00 177.40   0.80    2.00    --  111.00  61.00  90.00  118
 41  ω     87.00 177.40   0.80    2.00    --  111.00  30.00   0.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1095121000
_diffrn_orient_matrix_UB_12      -0.0444858000
_diffrn_orient_matrix_UB_13      0.0732184000
_diffrn_orient_matrix_UB_21      -0.0982860000
_diffrn_orient_matrix_UB_22      -0.1440475000
_diffrn_orient_matrix_UB_23      -0.0913758000
_diffrn_orient_matrix_UB_31      0.0828264000
_diffrn_orient_matrix_UB_32      0.0279166000
_diffrn_orient_matrix_UB_33      -0.0740573000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5213
_reflns_number_total             5341

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00164(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5341
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0198
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+0.7159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0566
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O10-H10A = O10-H10B = O4-H4B = O4-H4A
 0.82 with sigma of 0.01
 O14-H14B = O14-H14A = O15-H15B = O15-H15A
 0.82 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C14(H14), C16(H16), C17(H17)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
C1 C 0.6253(3) 0.8902(3) 0.9655(3) 0.0203(6) Uani 1 1 d . . . . .
C2 C 0.5204(3) 0.6880(3) 0.7595(3) 0.0149(5) Uani 1 1 d . . . . .
C3 C 0.5773(3) 0.6457(3) 0.9589(2) 0.0170(5) Uani 1 1 d . . . . .
C4 C 0.2068(3) 0.4344(2) 0.6902(2) 0.0140(5) Uani 1 1 d . . . . .
H4 H 0.257415 0.447231 0.643695 0.017 Uiso 1 1 calc R U . . .
C5 C 0.0839(3) 0.3145(3) 0.6488(2) 0.0160(5) Uani 1 1 d . . . . .
C6 C 0.0070(3) 0.2936(3) 0.7150(2) 0.0165(5) Uani 1 1 d . . . . .
H6 H -0.076664 0.211718 0.688223 0.020 Uiso 1 1 calc R U . . .
C7 C 0.0569(3) 0.3966(3) 0.8214(2) 0.0157(5) Uani 1 1 d . . . . .
H7 H 0.007003 0.386614 0.868647 0.019 Uiso 1 1 calc R U . . .
C8 C 0.1799(3) 0.5137(2) 0.8579(2) 0.0108(4) Uani 1 1 d . . . . .
C9 C 0.2431(3) 0.6310(2) 0.9729(2) 0.0132(5) Uani 1 1 d . . . . .
C10 C 0.0419(3) 0.2143(3) 0.5354(3) 0.0242(6) Uani 1 1 d . . . . .
H4A H 0.349(4) 0.8680(13) 0.795(4) 0.036 Uiso 1 1 d D U . . .
H4B H 0.276(4) 0.754(4) 0.7078(12) 0.036 Uiso 1 1 d D U . . .
H10A H 0.671(4) 0.1374(12) 0.716(4) 0.036 Uiso 1 1 d D U . . .
H10B H 0.730(4) 0.255(4) 0.8012(13) 0.036 Uiso 1 1 d D U . . .
C11 C 0.3780(3) 0.0942(3) 0.5513(3) 0.0174(5) Uani 1 1 d . . . . .
C12 C 0.4722(3) 0.3020(3) 0.7397(3) 0.0157(5) Uani 1 1 d . . . . .
C13 C 0.4096(3) 0.3325(3) 0.5349(2) 0.0164(5) Uani 1 1 d . . . . .
C14 C 0.7858(3) 0.5598(3) 0.7991(2) 0.0143(5) Uani 1 1 d . . . . .
H14 H 0.735525 0.551391 0.846143 0.017 Uiso 1 1 calc R U . . .
C15 C 0.9105(3) 0.6764(2) 0.8376(2) 0.0156(5) Uani 1 1 d . . . . .
C16 C 0.9869(3) 0.6919(3) 0.7707(2) 0.0166(5) Uani 1 1 d . . . . .
H16 H 1.071822 0.772046 0.795901 0.020 Uiso 1 1 calc R U . . .
C17 C 0.9338(3) 0.5854(3) 0.6655(2) 0.0154(5) Uani 1 1 d . . . . .
H17 H 0.982933 0.591076 0.617504 0.019 Uiso 1 1 calc R U . . .
C18 C 0.8096(3) 0.4718(2) 0.6320(2) 0.0111(4) Uani 1 1 d . . . . .
C19 C 0.7441(3) 0.3508(2) 0.5192(2) 0.0122(4) Uani 1 1 d . . . . .
C20 C 0.9574(4) 0.7802(3) 0.9499(3) 0.0274(6) Uani 1 1 d . . . . .
N1 N 0.2559(2) 0.5324(2) 0.7940(2) 0.0110(4) Uani 1 1 d . . . . .
N2 N 0.0175(4) 0.1429(3) 0.4481(3) 0.0392(7) Uani 1 1 d . . . . .
N3 N 0.7344(2) 0.4586(2) 0.6970(2) 0.0109(4) Uani 1 1 d . . . . .
N4 N 0.9884(4) 0.8556(3) 1.0373(3) 0.0428(8) Uani 1 1 d . . . . .
O1 O 0.7254(2) 0.9904(2) 1.0201(2) 0.0354(5) Uani 1 1 d . . . . .
O2 O 0.5591(2) 0.6645(2) 0.68847(19) 0.0265(4) Uani 1 1 d . . . . .
O3 O 0.6541(2) 0.6029(2) 1.00243(19) 0.0255(4) Uani 1 1 d . . . . .
O4 O 0.3036(2) 0.78842(19) 0.77950(18) 0.0142(4) Uani 1 1 d D . . . .
O5 O 0.1835(2) 0.62273(19) 1.03791(16) 0.0178(4) Uani 1 1 d . . . . .
O6 O 0.3560(2) 0.73126(19) 0.99240(17) 0.0148(4) Uani 1 1 d . . . . .
O7 O 0.2830(2) -0.0096(2) 0.50842(19) 0.0298(5) Uani 1 1 d . . . . .
O8 O 0.4258(3) 0.3212(2) 0.8061(2) 0.0293(5) Uani 1 1 d . . . . .
O9 O 0.3317(2) 0.3725(2) 0.48812(18) 0.0250(4) Uani 1 1 d . . . . .
O10 O 0.7050(2) 0.21793(19) 0.73055(17) 0.0134(4) Uani 1 1 d D . . . .
O11 O 0.8023(2) 0.35753(19) 0.45309(17) 0.0183(4) Uani 1 1 d . . . . .
O12 O 0.6325(2) 0.25112(19) 0.50325(17) 0.0141(4) Uani 1 1 d . . . . .
O13 O 0.5364(2) 0.96812(17) 1.18852(16) 0.0283(4) Uani 1 1 d . . . . .
H13A H 0.479(3) 0.986(3) 1.218(3) 0.042 Uiso 1 1 d . U . . .
H13B H 0.488(4) 0.898(4) 1.131(3) 0.042 Uiso 1 1 d . U . . .
O14 O 0.61789(19) 0.96178(16) 0.69785(14) 0.0227(3) Uani 1 1 d D . . . .
H14A H 0.540(2) 0.904(3) 0.640(2) 0.034 Uiso 1 1 d D U . . .
H14B H 0.686(2) 0.941(3) 0.708(3) 0.034 Uiso 1 1 d D U . . .
O15 O 0.8668(2) 0.9298(3) 0.73322(19) 0.0493(6) Uani 1 1 d D . . . .
H15A H 0.911(4) 0.934(5) 0.692(3) 0.074 Uiso 1 1 d D U . . .
H15B H 0.937(3) 0.992(3) 0.794(2) 0.074 Uiso 1 1 d D U . . .
Re1 Re 0.45589(2) 0.71761(2) 0.87707(2) 0.01041(6) Uani 1 1 d . . . . .
Re2 Re 0.53922(2) 0.27118(2) 0.62403(2) 0.00977(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
C1 O1 1.134(4) . ?
C1 Re1 1.937(3) . ?
C2 O2 1.156(4) . ?
C2 Re1 1.899(3) . ?
C3 O3 1.145(4) . ?
C3 Re1 1.905(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(4) . ?
C4 N1 1.340(3) . ?
C5 C6 1.395(4) . ?
C5 C10 1.460(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(4) . ?
C8 C9 1.516(3) . ?
C8 N1 1.361(3) . ?
C9 O5 1.229(3) . ?
C9 O6 1.271(3) . ?
C10 N2 1.123(4) . ?
C11 O7 1.136(4) . ?
C11 Re2 1.935(3) . ?
C12 O8 1.158(4) . ?
C12 Re2 1.899(3) . ?
C13 O9 1.142(4) . ?
C13 Re2 1.909(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(4) . ?
C14 N3 1.339(3) . ?
C15 C16 1.394(4) . ?
C15 C20 1.455(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.375(4) . ?
C18 C19 1.517(3) . ?
C18 N3 1.361(3) . ?
C19 O11 1.230(3) . ?
C19 O12 1.275(3) . ?
C20 N4 1.120(4) . ?
N1 Re1 2.171(2) . ?
N3 Re2 2.172(2) . ?
O4 H4A 0.820(10) . ?
O4 H4B 0.817(10) . ?
O4 Re1 2.1960(19) . ?
O6 Re1 2.1427(19) . ?
O10 H10A 0.822(10) . ?
O10 H10B 0.814(10) . ?
O10 Re2 2.1973(19) . ?
O12 Re2 2.155(2) . ?
O13 H13A 0.90(3) . ?
O13 H13B 0.82(4) . ?
O14 H14A 0.825(10) . ?
O14 H14B 0.827(10) . ?
O15 H15A 0.828(10) . ?
O15 H15B 0.828(10) . ?

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
O1 C1 Re1 178.1(3) . . ?
O2 C2 Re1 176.9(2) . . ?
O3 C3 Re1 175.2(2) . . ?
C5 C4 H4 119.1 . . ?
N1 C4 H4 119.1 . . ?
N1 C4 C5 121.8(2) . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 C10 116.9(2) . . ?
C6 C5 C10 122.9(3) . . ?
C5 C6 H6 121.1 . . ?
C7 C6 C5 117.7(2) . . ?
C7 C6 H6 121.1 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 C9 123.2(2) . . ?
N1 C8 C7 122.5(2) . . ?
N1 C8 C9 114.3(2) . . ?
O5 C9 C8 119.1(2) . . ?
O5 C9 O6 125.9(2) . . ?
O6 C9 C8 115.0(2) . . ?
N2 C10 C5 175.4(3) . . ?
O7 C11 Re2 179.8(3) . . ?
O8 C12 Re2 176.7(3) . . ?
O9 C13 Re2 175.7(2) . . ?
C15 C14 H14 119.3 . . ?
N3 C14 H14 119.3 . . ?
N3 C14 C15 121.5(2) . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 C20 117.2(2) . . ?
C16 C15 C20 122.1(2) . . ?
C15 C16 H16 121.3 . . ?
C15 C16 C17 117.4(2) . . ?
C17 C16 H16 121.3 . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 122.9(2) . . ?
N3 C18 C17 122.9(2) . . ?
N3 C18 C19 114.2(2) . . ?
O11 C19 C18 118.0(2) . . ?
O11 C19 O12 126.5(2) . . ?
O12 C19 C18 115.5(2) . . ?
N4 C20 C15 176.4(4) . . ?
C4 N1 C8 118.3(2) . . ?
C4 N1 Re1 125.80(18) . . ?
C8 N1 Re1 115.77(16) . . ?
C14 N3 C18 118.3(2) . . ?
C14 N3 Re2 125.64(18) . . ?
C18 N3 Re2 116.06(17) . . ?
H4A O4 H4B 104(4) . . ?
Re1 O4 H4A 109(3) . . ?
Re1 O4 H4B 108(3) . . ?
C9 O6 Re1 119.79(16) . . ?
H10A O10 H10B 107(4) . . ?
Re2 O10 H10A 111(3) . . ?
Re2 O10 H10B 108(3) . . ?
C19 O12 Re2 119.20(16) . . ?
H13A O13 H13B 110(3) . . ?
H14A O14 H14B 112(3) . . ?
H15A O15 H15B 95(4) . . ?
C1 Re1 N1 172.57(10) . . ?
C1 Re1 O4 96.23(10) . . ?
C1 Re1 O6 98.01(10) . . ?
C2 Re1 C1 88.94(13) . . ?
C2 Re1 C3 85.93(12) . . ?
C2 Re1 N1 98.39(10) . . ?
C2 Re1 O4 95.10(10) . . ?
C2 Re1 O6 172.63(10) . . ?
C3 Re1 C1 87.32(12) . . ?
C3 Re1 N1 94.39(10) . . ?
C3 Re1 O4 176.31(9) . . ?
C3 Re1 O6 96.78(10) . . ?
N1 Re1 O4 81.96(8) . . ?
O6 Re1 N1 74.62(8) . . ?
O6 Re1 O4 81.78(8) . . ?
C11 Re2 N3 172.84(10) . . ?
C11 Re2 O10 95.80(10) . . ?
C11 Re2 O12 98.99(10) . . ?
C12 Re2 C11 85.72(12) . . ?
C12 Re2 C13 85.87(12) . . ?
C12 Re2 N3 100.46(11) . . ?
C12 Re2 O10 95.59(10) . . ?
C12 Re2 O12 175.10(9) . . ?
C13 Re2 C11 89.30(12) . . ?
C13 Re2 N3 94.72(10) . . ?
C13 Re2 O10 174.79(9) . . ?
C13 Re2 O12 95.49(10) . . ?
N3 Re2 O10 80.10(8) . . ?
O12 Re2 N3 74.76(8) . . ?
O12 Re2 O10 82.64(7) . . ?

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
O4 H4A O13 0.820(10) 1.793(13) 2.602(3) 169(4) 2_677 yes
O4 H4B O11 0.817(10) 1.881(13) 2.687(3) 169(4) 2_666 yes
O10 H10A O14 0.822(10) 1.840(12) 2.656(3) 172(4) 1_545 yes
O10 H10B O5 0.814(10) 1.911(14) 2.708(3) 166(4) 2_667 yes
C16 H16 O4 0.95 2.57 3.215(3) 125.6 1_655 yes
O13 H13A O14 0.90(3) 1.91(3) 2.797(2) 172(3) 2_677 yes
O13 H13B O6 0.82(4) 1.95(4) 2.766(3) 174(3) . yes
O14 H14A O12 0.825(10) 2.006(12) 2.825(3) 172(3) 2_666 yes
O14 H14B O15 0.827(10) 1.942(12) 2.757(3) 168(3) . yes
O15 H15A N2 0.828(10) 2.34(2) 3.122(4) 158(4) 2_666 yes
O15 H15B N4 0.828(10) 2.15(2) 2.883(4) 148(4) 2_777 yes

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
C4 C5 C6 C7 0.7(4) . . . . ?
C5 C4 N1 C8 -1.7(4) . . . . ?
C5 C4 N1 Re1 174.54(19) . . . . ?
C5 C6 C7 C8 -0.7(4) . . . . ?
C6 C7 C8 C9 -179.6(2) . . . . ?
C6 C7 C8 N1 -0.6(4) . . . . ?
C7 C8 C9 O5 0.3(4) . . . . ?
C7 C8 C9 O6 -179.5(2) . . . . ?
C7 C8 N1 C4 1.7(4) . . . . ?
C7 C8 N1 Re1 -174.85(19) . . . . ?
C8 C9 O6 Re1 -6.7(3) . . . . ?
C9 C8 N1 C4 -179.2(2) . . . . ?
C9 C8 N1 Re1 4.2(3) . . . . ?
C10 C5 C6 C7 -179.7(3) . . . . ?
C14 C15 C16 C17 -0.8(4) . . . . ?
C15 C14 N3 C18 1.1(4) . . . . ?
C15 C14 N3 Re2 -179.15(19) . . . . ?
C15 C16 C17 C18 0.7(4) . . . . ?
C16 C17 C18 C19 -179.8(2) . . . . ?
C16 C17 C18 N3 0.4(4) . . . . ?
C17 C18 C19 O11 -2.9(3) . . . . ?
C17 C18 C19 O12 177.0(2) . . . . ?
C17 C18 N3 C14 -1.3(4) . . . . ?
C17 C18 N3 Re2 178.94(19) . . . . ?
C18 C19 O12 Re2 5.9(3) . . . . ?
C19 C18 N3 C14 178.9(2) . . . . ?
C19 C18 N3 Re2 -0.9(3) . . . . ?
C20 C15 C16 C17 178.9(3) . . . . ?
N1 C4 C5 C6 0.5(4) . . . . ?
N1 C4 C5 C10 -179.1(2) . . . . ?
N1 C8 C9 O5 -178.8(2) . . . . ?
N1 C8 C9 O6 1.4(3) . . . . ?
N3 C14 C15 C16 -0.1(4) . . . . ?
N3 C14 C15 C20 -179.9(3) . . . . ?
N3 C18 C19 O11 176.9(2) . . . . ?
N3 C18 C19 O12 -3.2(3) . . . . ?
O5 C9 O6 Re1 173.5(2) . . . . ?
O11 C19 O12 Re2 -174.2(2) . . . . ?

