# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2166088'
loop_
_audit_author_name
_audit_author_address
A-B
;Nanchang University
China
;
_audit_update_record             
;
2022-04-12 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H28 Cl F2 N O9'
_chemical_formula_weight         463.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   15.475(2)
_cell_length_b                   9.1044(12)
_cell_length_c                   15.932(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.773(2)
_cell_angle_gamma                90
_cell_volume                     2197.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1865
_cell_measurement_theta_min      2.8570
_cell_measurement_theta_max      29.0840

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.238
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12928
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.344
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4979
_reflns_number_gt                2985
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4979
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0732
_refine_ls_wR_factor_ref         0.3006
_refine_ls_wR_factor_gt          0.2488
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O8 O 0.4554(6) 0.7293(10) 0.1895(4) 0.304(6) Uani 1 1 d . . . . .
O10 O 0.5451(8) 0.8852(11) 0.2090(6) 0.375(8) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 0.86486(13) 0.2500 0.0605(4) Uani 1 2 d S T P . .
O7 O 0.0671(4) 0.7787(6) 0.2328(3) 0.173(2) Uani 1 1 d . . . . .
O6 O -0.0306(3) 0.9497(4) 0.1768(2) 0.1237(13) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.80793(15) 0.2500 0.0724(4) Uani 1 2 d S T P . .
O2 O 0.78484(14) 0.6229(2) 0.02377(13) 0.0570(6) Uani 1 1 d . . . . .
O3 O 0.89391(16) 0.3729(3) 0.01488(16) 0.0670(7) Uani 1 1 d . . . . .
O5 O 0.66411(15) 0.2056(3) 0.04497(18) 0.0678(7) Uani 1 1 d . . . . .
O1 O 0.61414(15) 0.5054(3) 0.02737(15) 0.0641(7) Uani 1 1 d . . . . .
N1 N 0.71596(16) 0.3916(3) 0.90663(15) 0.0489(6) Uani 1 1 d . . . . .
H1A H 0.7454 0.4463 0.9494 0.073 Uiso 1 1 calc R U . . .
H1B H 0.7274 0.2971 0.9182 0.073 Uiso 1 1 calc R U . . .
H1C H 0.6583 0.4076 0.9008 0.073 Uiso 1 1 calc R U . . .
O4 O 0.79136(17) 0.1144(2) -0.04205(17) 0.0701(7) Uani 1 1 d . . . . .
C11 C 0.74400(19) 0.5942(3) 0.81175(17) 0.0485(7) Uani 1 1 d . . . . .
F2 F 0.59859(17) 0.6202(3) 0.82574(19) 0.1041(9) Uani 1 1 d . . . . .
C5 C 0.8788(2) 0.6264(4) 0.0427(3) 0.0703(10) Uani 1 1 d . . . . .
H5A H 0.8986 0.7035 0.0842 0.084 Uiso 1 1 calc R U . . .
H5B H 0.8996 0.6502 -0.0092 0.084 Uiso 1 1 calc R U . . .
C4 C 0.7448(3) 0.6394(4) 0.0961(2) 0.0634(9) Uani 1 1 d . . . . .
H4A H 0.7639 0.7302 0.1260 0.076 Uiso 1 1 calc R U . . .
H4B H 0.7608 0.5582 0.1356 0.076 Uiso 1 1 calc R U . . .
C12 C 0.6727(3) 0.6852(4) 0.8115(2) 0.0646(9) Uani 1 1 d . . . . .
C16 C 0.8181(2) 0.6668(5) 0.7963(2) 0.0661(9) Uani 1 1 d . . . . .
C3 C 0.6469(2) 0.6418(4) 0.0624(3) 0.0685(10) Uani 1 1 d . . . . .
H3A H 0.6175 0.6676 0.1086 0.082 Uiso 1 1 calc R U . . .
H3B H 0.6330 0.7170 0.0185 0.082 Uiso 1 1 calc R U . . .
C17 C 0.7438(3) 0.4310(4) 0.8265(2) 0.0636(9) Uani 1 1 d . . . . .
H17A H 0.7042 0.3848 0.7787 0.076 Uiso 1 1 calc R U . . .
H17B H 0.8026 0.3928 0.8283 0.076 Uiso 1 1 calc R U . . .
F1 F 0.88952(16) 0.5829(3) 0.79461(18) 0.1063(9) Uani 1 1 d . . . . .
C1 C 0.5804(2) 0.2559(5) 0.0536(3) 0.0753(11) Uani 1 1 d . . . . .
H1D H 0.5566 0.1924 0.0922 0.090 Uiso 1 1 calc R U . . .
H1E H 0.5401 0.2550 -0.0017 0.090 Uiso 1 1 calc R U . . .
C10 C 0.6624(3) 0.0618(4) 0.0124(3) 0.0834(12) Uani 1 1 d . . . . .
H10A H 0.6284 0.0584 -0.0459 0.100 Uiso 1 1 calc R U . . .
H10B H 0.6359 -0.0050 0.0473 0.100 Uiso 1 1 calc R U . . .
C8 C 0.8868(3) 0.1225(5) -0.0220(4) 0.0879(14) Uani 1 1 d . . . . .
H8A H 0.9077 0.1490 -0.0734 0.106 Uiso 1 1 calc R U . . .
H8B H 0.9105 0.0265 -0.0038 0.106 Uiso 1 1 calc R U . . .
C6 C 0.9189(2) 0.4832(5) 0.0776(2) 0.0763(11) Uani 1 1 d . . . . .
H6A H 0.9827 0.4917 0.0919 0.092 Uiso 1 1 calc R U . . .
H6B H 0.8983 0.4577 0.1293 0.092 Uiso 1 1 calc R U . . .
C2 C 0.5903(3) 0.4099(5) 0.0886(3) 0.0729(10) Uani 1 1 d . . . . .
H2A H 0.5351 0.4421 0.1024 0.087 Uiso 1 1 calc R U . . .
H2B H 0.6353 0.4120 0.1408 0.087 Uiso 1 1 calc R U . . .
C7 C 0.9200(2) 0.2307(5) 0.0460(3) 0.0771(11) Uani 1 1 d . . . . .
H7A H 0.8960 0.2097 0.0964 0.092 Uiso 1 1 calc R U . . .
H7B H 0.9838 0.2253 0.0620 0.092 Uiso 1 1 calc R U . . .
C9 C 0.7564(3) 0.0198(4) 0.0145(3) 0.0758(11) Uani 1 1 d . . . . .
H9A H 0.7908 0.0293 0.0724 0.091 Uiso 1 1 calc R U . . .
H9B H 0.7594 -0.0816 -0.0034 0.091 Uiso 1 1 calc R U . . .
C15 C 0.8197(4) 0.8150(6) 0.7813(3) 0.0998(17) Uani 1 1 d . . . . .
H15 H 0.8707 0.8601 0.7715 0.120 Uiso 1 1 calc R U . . .
C14 C 0.7450(6) 0.8951(6) 0.7809(3) 0.117(2) Uani 1 1 d . . . . .
H14 H 0.7448 0.9952 0.7693 0.140 Uiso 1 1 calc R U . . .
C13 C 0.6728(4) 0.8326(6) 0.7970(3) 0.1016(17) Uani 1 1 d . . . . .
H13 H 0.6229 0.8886 0.7984 0.122 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O8 Cl2 1.283(6) . ?
O10 Cl2 1.263(6) . ?
Cl1 O7 1.373(4) . ?
Cl1 O7 1.373(4) 2 ?
Cl1 O6 1.399(3) 2 ?
Cl1 O6 1.399(3) . ?
Cl2 O10 1.263(6) 2_655 ?
Cl2 O8 1.283(6) 2_655 ?
O2 C5 1.424(4) . ?
O2 C4 1.423(4) . ?
O3 C6 1.414(5) . ?
O3 C7 1.415(4) . ?
O5 C1 1.408(4) . ?
O5 C10 1.407(5) . ?
O1 C2 1.411(4) . ?
O1 C3 1.412(4) . ?
N1 C17 1.472(4) . ?
O4 C9 1.431(4) . ?
O4 C8 1.448(5) . ?
C11 C12 1.378(5) . ?
C11 C16 1.389(5) . ?
C11 C17 1.505(5) . ?
F2 C12 1.351(4) . ?
C5 C6 1.501(5) . ?
C4 C3 1.501(5) . ?
C12 C13 1.362(6) . ?
C16 F1 1.348(5) . ?
C16 C15 1.371(7) . ?
C1 C2 1.505(5) . ?
C10 C9 1.497(5) . ?
C8 C7 1.478(6) . ?
C15 C14 1.366(8) . ?
C14 C13 1.324(8) . ?

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
O7 Cl1 O7 110.3(6) . 2 ?
O7 Cl1 O6 110.0(3) . 2 ?
O7 Cl1 O6 106.8(3) 2 2 ?
O7 Cl1 O6 106.8(3) . . ?
O7 Cl1 O6 110.0(3) 2 . ?
O6 Cl1 O6 113.0(4) 2 . ?
O10 Cl2 O10 112.3(10) 2_655 . ?
O10 Cl2 O8 115.5(8) 2_655 . ?
O10 Cl2 O8 101.0(5) . . ?
O10 Cl2 O8 101.0(5) 2_655 2_655 ?
O10 Cl2 O8 115.5(8) . 2_655 ?
O8 Cl2 O8 112.2(8) . 2_655 ?
C5 O2 C4 114.9(3) . . ?
C6 O3 C7 112.6(3) . . ?
C1 O5 C10 113.0(3) . . ?
C2 O1 C3 113.1(3) . . ?
C9 O4 C8 113.1(3) . . ?
C12 C11 C16 113.7(3) . . ?
C12 C11 C17 124.5(3) . . ?
C16 C11 C17 121.8(3) . . ?
O2 C5 C6 112.7(3) . . ?
O2 C4 C3 106.7(3) . . ?
F2 C12 C11 116.3(3) . . ?
F2 C12 C13 119.4(4) . . ?
C11 C12 C13 124.3(4) . . ?
F1 C16 C15 120.7(4) . . ?
F1 C16 C11 116.3(4) . . ?
C15 C16 C11 123.0(4) . . ?
O1 C3 C4 112.5(3) . . ?
N1 C17 C11 112.7(3) . . ?
O5 C1 C2 108.2(3) . . ?
O5 C10 C9 106.5(3) . . ?
O4 C8 C7 112.4(3) . . ?
O3 C6 C5 108.8(3) . . ?
O1 C2 C1 109.8(3) . . ?
O3 C7 C8 108.7(3) . . ?
O4 C9 C10 108.8(3) . . ?
C14 C15 C16 118.7(5) . . ?
C13 C14 C15 121.1(5) . . ?
C14 C13 C12 119.1(5) . . ?

_refine_diff_density_max         0.582
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.062

####################################################################### 
# 
# 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_mm2
_database_code_depnum_ccdc_archive 'CCDC 2166089'
loop_
_audit_author_name
_audit_author_address
A-B
;Nanchang University
China
;
_audit_update_record             
;
2022-04-12 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H28 F2 N O9 Re'
_chemical_formula_weight         614.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   16.1750(12)
_cell_length_b                   9.2848(7)
_cell_length_c                   15.0120(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2254.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7157
_cell_measurement_theta_min      2.7260
_cell_measurement_theta_max      75.4230

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    5.452
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   multi-scan
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12989
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.518
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_point_group_measured_fraction_full 0.908
_reflns_number_total             4603
_reflns_number_gt                3509
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_max     0.767
_reflns_Friedel_fraction_full    0.808

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1212 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4603
_refine_ls_number_parameters     272
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.905
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.20404(2) 0.63058(2) 0.39002(7) 0.04334(9) Uani 1 1 d . . . . .
O4 O 0.1784(6) 0.4556(8) 0.4032(9) 0.130(3) Uani 1 1 d . . . . .
O1 O 0.2141(5) 0.6618(9) 0.2768(5) 0.097(3) Uani 1 1 d . . . . .
O3 O 0.1288(5) 0.7390(11) 0.4324(5) 0.109(3) Uani 1 1 d . . . . .
O2 O 0.2938(5) 0.6606(12) 0.4439(8) 0.125(4) Uani 1 1 d . . . . .
N1 N 0.4160(3) -0.1546(6) 0.1067(4) 0.0404(14) Uani 1 1 d . . . . .
H1A H 0.4175 -0.1533 0.0475 0.061 Uiso 1 1 calc R U . . .
H1B H 0.4311 -0.2412 0.1262 0.061 Uiso 1 1 calc R U . . .
H1C H 0.4504 -0.0883 0.1281 0.061 Uiso 1 1 calc R U . . .
O6 O 0.5609(4) 0.6605(7) 0.0585(5) 0.0706(18) Uani 1 1 d . . . . .
O7 O 0.5528(4) 0.9515(8) -0.0005(5) 0.0697(18) Uani 1 1 d . . . . .
O8 O 0.5195(4) 1.0808(6) 0.1664(5) 0.0692(17) Uani 1 1 d . . . . .
O9 O 0.4911(4) 0.8432(8) 0.2823(4) 0.079(2) Uani 1 1 d . . . . .
F1 F 0.2757(3) -0.0033(7) 0.2992(4) 0.0843(16) Uani 1 1 d . . . . .
O5 O 0.4519(4) 0.5782(7) 0.1892(6) 0.080(2) Uani 1 1 d . . . . .
C8 C 0.3159(4) 0.0361(8) 0.1509(6) 0.0419(17) Uani 1 1 d . . . . .
C10 C 0.6196(7) 0.8565(11) -0.0168(9) 0.086(3) Uani 1 1 d . . . . .
H10A H 0.6590 0.8624 0.0318 0.103 Uiso 1 1 calc R U . . .
H10B H 0.6476 0.8843 -0.0713 0.103 Uiso 1 1 calc R U . . .
C11 C 0.5139(9) 0.7068(17) 0.3141(8) 0.110(4) Uani 1 1 d . . . . .
H11A H 0.5148 0.7079 0.3787 0.132 Uiso 1 1 calc R U . . .
H11B H 0.5690 0.6832 0.2932 0.132 Uiso 1 1 calc R U . . .
C12 C 0.3299(5) -0.1225(8) 0.1376(7) 0.056(2) Uani 1 1 d . . . . .
H12A H 0.3198 -0.1724 0.1934 0.067 Uiso 1 1 calc R U . . .
H12B H 0.2908 -0.1586 0.0941 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5886(6) 0.7073(14) -0.0250(7) 0.084(3) Uani 1 1 d . . . . .
H13A H 0.5437 0.7037 -0.0677 0.100 Uiso 1 1 calc R U . . .
H13B H 0.6325 0.6447 -0.0460 0.100 Uiso 1 1 calc R U . . .
C14 C 0.5785(7) 1.0904(11) 0.0260(9) 0.088(4) Uani 1 1 d . . . . .
H14A H 0.5357 1.1595 0.0110 0.106 Uiso 1 1 calc R U . . .
H14B H 0.6280 1.1165 -0.0068 0.106 Uiso 1 1 calc R U . . .
C17 C 0.2722(6) 0.2335(13) 0.2456(8) 0.075(3) Uani 1 1 d . . . . .
H17 H 0.2525 0.2651 0.3004 0.091 Uiso 1 1 calc R U . . .
C18 C 0.5143(7) 0.4830(10) 0.1556(10) 0.087(4) Uani 1 1 d . . . . .
H18A H 0.5645 0.4934 0.1903 0.105 Uiso 1 1 calc R U . . .
H18B H 0.4957 0.3840 0.1605 0.105 Uiso 1 1 calc R U . . .
C19 C 0.5307(7) 0.5183(11) 0.0618(10) 0.088(4) Uani 1 1 d . . . . .
H19A H 0.4803 0.5103 0.0272 0.106 Uiso 1 1 calc R U . . .
H19B H 0.5712 0.4523 0.0373 0.106 Uiso 1 1 calc R U . . .
C21 C 0.2850(6) 0.3264(12) 0.1791(11) 0.084(4) Uani 1 1 d . . . . .
H21 H 0.2748 0.4237 0.1886 0.101 Uiso 1 1 calc R U . . .
C22 C 0.4531(10) 0.5939(16) 0.2819(10) 0.117(5) Uani 1 1 d . . . . .
H22A H 0.4673 0.5020 0.3087 0.140 Uiso 1 1 calc R U . . .
H22B H 0.3981 0.6197 0.3022 0.140 Uiso 1 1 calc R U . . .
C24 C 0.5960(6) 1.0988(9) 0.1236(9) 0.078(3) Uani 1 1 d . . . . .
H24A H 0.6342 1.0235 0.1413 0.094 Uiso 1 1 calc R U . . .
H24B H 0.6200 1.1914 0.1387 0.094 Uiso 1 1 calc R U . . .
C26 C 0.5511(6) 0.9505(16) 0.3006(7) 0.093(4) Uani 1 1 d . . . . .
H26A H 0.6042 0.9217 0.2764 0.112 Uiso 1 1 calc R U . . .
H26B H 0.5570 0.9623 0.3645 0.112 Uiso 1 1 calc R U . . .
C34 C 0.5245(8) 1.0876(14) 0.2600(9) 0.095(4) Uani 1 1 d . . . . .
H34A H 0.4708 1.1139 0.2837 0.114 Uiso 1 1 calc R U . . .
H34B H 0.5634 1.1626 0.2765 0.114 Uiso 1 1 calc R U . . .
C30 C 0.3268(6) 0.1366(9) 0.0856(7) 0.056(2) Uani 1 1 d . . . . .
F2 F 0.3525(4) 0.0860(7) 0.0059(4) 0.0909(19) Uani 1 1 d . . . . .
C33 C 0.2888(5) 0.0902(11) 0.2313(7) 0.056(2) Uani 1 1 d . . . . .
C35 C 0.3134(6) 0.2814(11) 0.0958(9) 0.081(3) Uani 1 1 d . . . . .
H35 H 0.3227 0.3463 0.0496 0.097 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O2 1.685(8) . ?
Re1 O4 1.688(7) . ?
Re1 O3 1.703(7) . ?
Re1 O1 1.731(8) . ?
N1 C12 1.497(10) . ?
O6 C13 1.400(12) . ?
O6 C19 1.409(11) . ?
O7 C10 1.416(12) . ?
O7 C14 1.413(12) . ?
O8 C24 1.404(13) . ?
O8 C34 1.409(14) . ?
O9 C11 1.402(13) . ?
O9 C26 1.418(13) . ?
F1 C33 1.355(11) . ?
O5 C22 1.399(17) . ?
O5 C18 1.433(12) . ?
C8 C30 1.364(12) . ?
C8 C33 1.380(12) . ?
C8 C12 1.503(9) . ?
C10 C13 1.479(14) . ?
C11 C22 1.52(2) . ?
C14 C24 1.495(17) . ?
C17 C21 1.336(17) . ?
C17 C33 1.374(14) . ?
C18 C19 1.471(18) . ?
C21 C35 1.396(18) . ?
C26 C34 1.476(17) . ?
C30 F2 1.351(11) . ?
C30 C35 1.371(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Re1 O4 108.4(6) . . ?
O2 Re1 O3 109.8(5) . . ?
O4 Re1 O3 110.4(5) . . ?
O2 Re1 O1 111.2(6) . . ?
O4 Re1 O1 107.4(6) . . ?
O3 Re1 O1 109.6(4) . . ?
C13 O6 C19 115.7(9) . . ?
C10 O7 C14 113.1(9) . . ?
C24 O8 C34 113.5(8) . . ?
C11 O9 C26 112.8(10) . . ?
C22 O5 C18 113.8(10) . . ?
C30 C8 C33 114.9(8) . . ?
C30 C8 C12 123.8(8) . . ?
C33 C8 C12 121.3(8) . . ?
O7 C10 C13 109.8(9) . . ?
O9 C11 C22 110.2(10) . . ?
N1 C12 C8 112.1(6) . . ?
O6 C13 C10 109.0(9) . . ?
O7 C14 C24 112.3(8) . . ?
C21 C17 C33 118.5(10) . . ?
C19 C18 O5 109.1(8) . . ?
C18 C19 O6 107.8(10) . . ?
C17 C21 C35 121.9(10) . . ?
O5 C22 C11 113.4(9) . . ?
O8 C24 C14 106.0(9) . . ?
O9 C26 C34 109.1(9) . . ?
O8 C34 C26 113.0(9) . . ?
F2 C30 C8 115.9(7) . . ?
F2 C30 C35 119.2(9) . . ?
C8 C30 C35 124.8(10) . . ?
F1 C33 C8 118.4(8) . . ?
F1 C33 C17 118.2(9) . . ?
C8 C33 C17 123.5(10) . . ?
C30 C35 C21 116.4(10) . . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.103

