# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1908117'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2019-04-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C15 H14 Cl N4 O3 Re, C3 H7 N O'
_chemical_formula_sum            'C18 H21 Cl N5 O4 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         593.05

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   8.953(3)
_cell_length_b                   9.085(3)
_cell_length_c                   13.399(4)
_cell_angle_alpha                80.373(4)
_cell_angle_beta                 76.566(4)
_cell_angle_gamma                78.668(4)
_cell_volume                     1030.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9351
_cell_measurement_theta_min      2.3711
_cell_measurement_theta_max      30.5141
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.085
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576

_exptl_absorpt_coefficient_mu    6.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_T_max  0.63

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            25548
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_full        30.59
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19

_refine_special_details          
;
;

_reflns_number_total             6210
_reflns_number_gt                5716
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0501
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.069
_refine_ls_number_reflns         6210
_refine_ls_number_parameters     272
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+0.5921P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.972
_refine_diff_density_min         -1.081
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.2222(3) 0.9053(3) 0.47510(19) 0.0150(5) Uani d . . . 1 . .
C C2 0.1756(3) 1.0379(3) 0.4099(2) 0.0192(5) Uani d . . . 1 . .
H H2 0.1336 1.0312 0.3522 0.023 Uiso calc U . R 1 . .
C C3 0.1918(3) 1.1756(3) 0.4307(2) 0.0212(6) Uani d . . . 1 . .
H H3 0.1598 1.2654 0.388 0.025 Uiso calc U . R 1 . .
C C4 0.2554(3) 1.1839(3) 0.5148(2) 0.0186(5) Uani d . . . 1 . .
H H4 0.2695 1.2787 0.5289 0.022 Uiso calc U . R 1 . .
C C5 0.2974(3) 1.0525(3) 0.57719(19) 0.0131(5) Uani d . . . 1 . .
C C6 0.3724(3) 1.0525(3) 0.6646(2) 0.0145(5) Uani d . . . 1 . .
C C7 0.4026(3) 1.1847(3) 0.6884(2) 0.0193(5) Uani d . . . 1 . .
H H7 0.3718 1.2794 0.6503 0.023 Uiso calc U . R 1 . .
C C8 0.4790(3) 1.1767(3) 0.7692(2) 0.0221(6) Uani d . . . 1 . .
H H8 0.4951 1.2667 0.7895 0.027 Uiso calc U . R 1 . .
C C9 0.5303(3) 1.0392(3) 0.8188(2) 0.0202(5) Uani d . . . 1 . .
H H9 0.5864 1.0326 0.8719 0.024 Uiso calc U . R 1 . .
C C10 0.4998(3) 0.9051(3) 0.7910(2) 0.0158(5) Uani d . . . 1 . .
C C11 0.1489(3) 0.7438(4) 0.3688(2) 0.0226(6) Uani d . . . 1 . .
H H11A 0.14 0.637 0.3733 0.034 Uiso calc U . R 1 . .
H H11B 0.2193 0.7736 0.3039 0.034 Uiso calc U . R 1 . .
H H11C 0.046 0.8062 0.3708 0.034 Uiso calc U . R 1 . .
C C12 0.6456(4) 0.7499(4) 0.9175(2) 0.0262(6) Uani d . . . 1 . .
H H12A 0.6517 0.6464 0.9535 0.039 Uiso calc U . R 1 . .
H H12B 0.5953 0.8216 0.9671 0.039 Uiso calc U . R 1 . .
H H12C 0.7509 0.7704 0.8855 0.039 Uiso calc U . R 1 . .
C C13 0.2933(3) 0.6062(3) 0.8218(2) 0.0179(5) Uani d . . . 1 . .
C C14 0.4769(3) 0.6096(3) 0.6265(2) 0.0163(5) Uani d . . . 1 . .
C C15 0.1708(3) 0.6053(3) 0.6655(2) 0.0169(5) Uani d . . . 1 . .
O O1 0.2826(3) 0.5280(2) 0.89928(16) 0.0267(5) Uani d . . . 1 . .
O O2 0.5824(3) 0.5264(2) 0.58844(17) 0.0265(5) Uani d . . . 1 . .
O O3 0.0966(3) 0.5219(2) 0.65241(17) 0.0257(4) Uani d . . . 1 . .
Cl Cl1 0.05897(7) 0.89764(7) 0.78209(4) 0.01407(11) Uani d . . . 1 . .
Re Re1 0.29666(2) 0.73659(2) 0.69199(2) 0.01157(3) Uani d . . . 1 . .
N N1 0.2776(2) 0.9139(2) 0.56045(16) 0.0133(4) Uani d . . . 1 . .
N N2 0.4142(2) 0.9142(2) 0.71763(16) 0.0129(4) Uani d . . . 1 . .
N N3 0.2096(3) 0.7653(3) 0.45428(17) 0.0158(4) Uani d . . D 1 . .
H H1N 0.273(3) 0.696(3) 0.479(2) 0.019 Uiso d U . D 1 . .
N N4 0.5546(3) 0.7669(3) 0.83725(18) 0.0199(5) Uani d . . D 1 . .
H H2N 0.564(4) 0.679(2) 0.822(3) 0.024 Uiso d U . D 1 . .
C C16 0.7918(4) 0.1611(4) 0.9631(3) 0.0303(7) Uani d . . . 1 . .
H H16A 0.6795 0.1897 0.9662 0.046 Uiso calc U . R 1 . .
H H16B 0.8119 0.1441 1.0333 0.046 Uiso calc U . R 1 . .
H H16C 0.8302 0.068 0.9307 0.046 Uiso calc U . R 1 . .
C C17 1.0370(4) 0.2659(5) 0.9021(3) 0.0405(9) Uani d . . . 1 . .
H H17A 1.0801 0.3497 0.8557 0.061 Uiso calc U . R 1 . .
H H17B 1.0914 0.1696 0.878 0.061 Uiso calc U . R 1 . .
H H17C 1.0506 0.2678 0.9723 0.061 Uiso calc U . R 1 . .
C C18 0.7950(4) 0.4015(4) 0.8521(2) 0.0302(7) Uani d . . . 1 . .
H H18 0.8536 0.4779 0.8161 0.036 Uiso calc U . R 1 . .
N N5 0.8711(3) 0.2816(3) 0.9024(2) 0.0259(5) Uani d . . . 1 . .
O O4 0.6563(3) 0.4228(3) 0.8476(2) 0.0362(6) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.367(3) ?
C1 N3 . 1.378(3) ?
C1 C2 . 1.418(4) ?
C2 C3 . 1.368(4) ?
C2 H2 . 0.95 ?
C3 C4 . 1.393(4) ?
C3 H3 . 0.95 ?
C4 C5 . 1.379(4) ?
C4 H4 . 0.95 ?
C5 N1 . 1.368(3) ?
C5 C6 . 1.479(3) ?
C6 N2 . 1.365(3) ?
C6 C7 . 1.383(3) ?
C7 C8 . 1.394(4) ?
C7 H7 . 0.95 ?
C8 C9 . 1.361(4) ?
C8 H8 . 0.95 ?
C9 C10 . 1.423(4) ?
C9 H9 . 0.95 ?
C10 N4 . 1.357(4) ?
C10 N2 . 1.363(3) ?
C11 N3 . 1.431(3) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 N4 . 1.465(3) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 O1 . 1.152(3) ?
C13 Re1 . 1.931(3) ?
C14 O2 . 1.160(3) ?
C14 Re1 . 1.912(3) ?
C15 O3 . 1.159(3) ?
C15 Re1 . 1.917(3) ?
Cl1 Re1 . 2.5100(7) ?
Re1 N1 . 2.194(2) ?
Re1 N2 . 2.202(2) ?
N3 H1N . 0.838(18) ?
N4 H2N . 0.840(18) ?
C16 N5 . 1.450(4) ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 N5 . 1.463(4) ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 O4 . 1.233(4) ?
C18 N5 . 1.335(4) ?
C18 H18 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 N3 . . 118.9(2) ?
N1 C1 C2 . . 120.9(2) ?
N3 C1 C2 . . 120.3(2) ?
C3 C2 C1 . . 119.4(3) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
C2 C3 C4 . . 119.8(3) ?
C2 C3 H3 . . 120.1 ?
C4 C3 H3 . . 120.1 ?
C5 C4 C3 . . 119.1(3) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
N1 C5 C4 . . 122.5(2) ?
N1 C5 C6 . . 115.7(2) ?
C4 C5 C6 . . 121.8(2) ?
N2 C6 C7 . . 122.4(2) ?
N2 C6 C5 . . 116.0(2) ?
C7 C6 C5 . . 121.6(2) ?
C6 C7 C8 . . 118.9(3) ?
C6 C7 H7 . . 120.5 ?
C8 C7 H7 . . 120.5 ?
C9 C8 C7 . . 119.6(2) ?
C9 C8 H8 . . 120.2 ?
C7 C8 H8 . . 120.2 ?
C8 C9 C10 . . 119.9(3) ?
C8 C9 H9 . . 120.1 ?
C10 C9 H9 . . 120.1 ?
N4 C10 N2 . . 119.1(2) ?
N4 C10 C9 . . 120.7(2) ?
N2 C10 C9 . . 120.3(2) ?
N3 C11 H11A . . 109.5 ?
N3 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
N3 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
N4 C12 H12A . . 109.5 ?
N4 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N4 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
O1 C13 Re1 . . 176.1(2) ?
O2 C14 Re1 . . 176.6(2) ?
O3 C15 Re1 . . 177.4(2) ?
C14 Re1 C15 . . 88.64(11) ?
C14 Re1 C13 . . 91.25(11) ?
C15 Re1 C13 . . 84.27(11) ?
C14 Re1 N1 . . 97.67(10) ?
C15 Re1 N1 . . 99.42(10) ?
C13 Re1 N1 . . 170.40(9) ?
C14 Re1 N2 . . 97.94(10) ?
C15 Re1 N2 . . 171.73(9) ?
C13 Re1 N2 . . 100.51(10) ?
N1 Re1 N2 . . 74.83(8) ?
C14 Re1 Cl1 . . 178.42(8) ?
C15 Re1 Cl1 . . 90.82(8) ?
C13 Re1 Cl1 . . 87.22(9) ?
N1 Re1 Cl1 . . 83.88(6) ?
N2 Re1 Cl1 . . 82.73(6) ?
C1 N1 C5 . . 118.3(2) ?
C1 N1 Re1 . . 126.51(17) ?
C5 N1 Re1 . . 114.09(16) ?
C10 N2 C6 . . 118.5(2) ?
C10 N2 Re1 . . 126.81(17) ?
C6 N2 Re1 . . 113.68(16) ?
C1 N3 C11 . . 123.4(2) ?
C1 N3 H1N . . 112.(2) ?
C11 N3 H1N . . 120.(2) ?
C10 N4 C12 . . 121.6(2) ?
C10 N4 H2N . . 133.(2) ?
C12 N4 H2N . . 105.(2) ?
N5 C16 H16A . . 109.5 ?
N5 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
N5 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
N5 C17 H17A . . 109.5 ?
N5 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
N5 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
O4 C18 N5 . . 126.4(3) ?
O4 C18 H18 . . 116.8 ?
N5 C18 H18 . . 116.8 ?
C18 N5 C16 . . 121.4(3) ?
C18 N5 C17 . . 122.3(3) ?
C16 N5 C17 . . 116.3(3) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 C3 . . . . 2.4(4) ?
N3 C1 C2 C3 . . . . -178.8(2) ?
C1 C2 C3 C4 . . . . 0.8(4) ?
C2 C3 C4 C5 . . . . -1.6(4) ?
C3 C4 C5 N1 . . . . -0.7(4) ?
C3 C4 C5 C6 . . . . 177.0(2) ?
N1 C5 C6 N2 . . . . 0.6(3) ?
C4 C5 C6 N2 . . . . -177.3(2) ?
N1 C5 C6 C7 . . . . 178.4(2) ?
C4 C5 C6 C7 . . . . 0.5(4) ?
N2 C6 C7 C8 . . . . 0.2(4) ?
C5 C6 C7 C8 . . . . -177.5(2) ?
C6 C7 C8 C9 . . . . 3.9(4) ?
C7 C8 C9 C10 . . . . -2.7(4) ?
C8 C9 C10 N4 . . . . 177.8(3) ?
C8 C9 C10 N2 . . . . -2.5(4) ?
N3 C1 N1 C5 . . . . 176.6(2) ?
C2 C1 N1 C5 . . . . -4.6(4) ?
N3 C1 N1 Re1 . . . . -16.3(3) ?
C2 C1 N1 Re1 . . . . 162.49(19) ?
C4 C5 N1 C1 . . . . 3.8(4) ?
C6 C5 N1 C1 . . . . -174.1(2) ?
C4 C5 N1 Re1 . . . . -164.8(2) ?
C6 C5 N1 Re1 . . . . 17.3(3) ?
N4 C10 N2 C6 . . . . -173.8(2) ?
C9 C10 N2 C6 . . . . 6.5(4) ?
N4 C10 N2 Re1 . . . . 18.2(3) ?
C9 C10 N2 Re1 . . . . -161.52(19) ?
C7 C6 N2 C10 . . . . -5.4(4) ?
C5 C6 N2 C10 . . . . 172.5(2) ?
C7 C6 N2 Re1 . . . . 164.1(2) ?
C5 C6 N2 Re1 . . . . -18.0(3) ?
N1 C1 N3 C11 . . . . 178.1(2) ?
C2 C1 N3 C11 . . . . -0.7(4) ?
N2 C10 N4 C12 . . . . -179.3(2) ?
C9 C10 N4 C12 . . . . 0.4(4) ?
O4 C18 N5 C16 . . . . -2.4(5) ?
O4 C18 N5 C17 . . . . 179.3(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_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1908120'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2019-04-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C15 H13 Cl N3 O3 Re'
_chemical_formula_sum            'C15 H13 Cl N3 O3 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         504.93

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   7.333(2)
_cell_length_b                   8.821(3)
_cell_length_c                   13.059(4)
_cell_angle_alpha                91.690(4)
_cell_angle_beta                 99.041(4)
_cell_angle_gamma                107.903(4)
_cell_volume                     791.1(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    117
_cell_measurement_theta_min      3.1221
_cell_measurement_theta_max      29.7675
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear orange'
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.200
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480

_exptl_absorpt_coefficient_mu    7.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_T_max  0.30

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            19445
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;
;

_reflns_number_total             4782
_reflns_number_gt                4686
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0157
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0384
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_number_reflns         4782
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0114P)²+0.5504P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.947
_refine_diff_density_min         -1.237
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4288(3) 0.0767(2) 0.65934(16) 0.0146(4) Uani d . . . 1 . .
C C2 0.7772(3) 0.0544(2) 0.65299(17) 0.0160(4) Uani d . . . 1 . .
C C3 0.6664(3) 0.0950(2) 0.83974(17) 0.0141(4) Uani d . . . 1 . .
C C4 0.6224(3) 0.3329(3) 0.49513(16) 0.0141(4) Uani d . . . 1 . .
H H4 0.5302 0.2295 0.477 0.017 Uiso calc U . R 1 . .
C C5 0.6440(3) 0.4427(3) 0.42135(16) 0.0166(4) Uani d . . . 1 . .
H H5 0.5696 0.4151 0.3531 0.02 Uiso calc U . R 1 . .
C C6 0.7768(3) 0.5947(3) 0.44887(16) 0.0163(4) Uani d . . . 1 . .
H H6 0.792 0.6733 0.4 0.02 Uiso calc U . R 1 . .
C C7 0.8869(3) 0.6306(2) 0.54822(16) 0.0142(4) Uani d . . . 1 . .
H H7 0.9786 0.7339 0.5679 0.017 Uiso calc U . R 1 . .
C C8 0.8614(3) 0.5129(2) 0.61900(15) 0.0115(3) Uani d . . . 1 . .
C C9 0.9823(3) 0.5359(2) 0.72349(15) 0.0115(3) Uani d . . . 1 . .
C C10 1.1001(3) 0.6847(2) 0.76851(16) 0.0154(4) Uani d . . . 1 . .
H H10 1.1062 0.778 0.7328 0.018 Uiso calc U . R 1 . .
C C11 1.2098(3) 0.6949(3) 0.86730(17) 0.0174(4) Uani d . . . 1 . .
H H11 1.2857 0.7965 0.9014 0.021 Uiso calc U . R 1 . .
C C12 1.2084(3) 0.5580(3) 0.91568(16) 0.0158(4) Uani d . . . 1 . .
H H12 1.284 0.5644 0.9827 0.019 Uiso calc U . R 1 . .
C C13 1.0927(3) 0.4073(2) 0.86423(15) 0.0116(3) Uani d . . . 1 . .
C C14 1.1211(3) 0.1393(2) 0.84091(17) 0.0162(4) Uani d . . . 1 . .
H H14A 1.1057 0.1636 0.7679 0.024 Uiso calc U . R 1 . .
H H14B 1.0231 0.0378 0.8485 0.024 Uiso calc U . R 1 . .
H H14C 1.2515 0.131 0.863 0.024 Uiso calc U . R 1 . .
C C15 1.1886(3) 0.2748(3) 1.01424(17) 0.0195(4) Uani d . . . 1 . .
H H15A 1.3302 0.3086 1.0188 0.029 Uiso calc U . R 1 . .
H H15B 1.1445 0.1689 1.0403 0.029 Uiso calc U . R 1 . .
H H15C 1.1532 0.3517 1.0563 0.029 Uiso calc U . R 1 . .
N N1 0.7278(2) 0.3670(2) 0.59247(13) 0.0112(3) Uani d . . . 1 . .
N N2 0.9707(2) 0.3983(2) 0.77233(13) 0.0107(3) Uani d . . . 1 . .
N N3 1.0958(2) 0.2676(2) 0.90583(13) 0.0134(3) Uani d . . . 1 . .
O O1 0.2734(2) -0.0028(2) 0.62437(13) 0.0219(3) Uani d . . . 1 . .
O O2 0.8230(3) -0.0448(2) 0.61528(15) 0.0267(4) Uani d . . . 1 . .
O O3 0.6486(2) 0.0272(2) 0.91380(13) 0.0218(3) Uani d . . . 1 . .
Cl Cl1 0.56112(7) 0.40734(6) 0.79644(4) 0.01361(9) Uani d . . . 1 . .
Re Re1 0.68737(2) 0.20925(2) 0.71644(2) 0.00930(3) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.152(3) ?
C1 Re1 . 1.913(2) ?
C2 O2 . 1.153(3) ?
C2 Re1 . 1.909(2) ?
C3 O3 . 1.156(3) ?
C3 Re1 . 1.926(2) ?
C4 N1 . 1.353(3) ?
C4 C5 . 1.379(3) ?
C4 H4 . 0.95 ?
C5 C6 . 1.391(3) ?
C5 H5 . 0.95 ?
C6 C7 . 1.388(3) ?
C6 H6 . 0.95 ?
C7 C8 . 1.400(3) ?
C7 H7 . 0.95 ?
C8 N1 . 1.352(3) ?
C8 C9 . 1.477(3) ?
C9 N2 . 1.373(3) ?
C9 C10 . 1.383(3) ?
C10 C11 . 1.393(3) ?
C10 H10 . 0.95 ?
C11 C12 . 1.377(3) ?
C11 H11 . 0.95 ?
C12 C13 . 1.418(3) ?
C12 H12 . 0.95 ?
C13 N2 . 1.364(3) ?
C13 N3 . 1.366(3) ?
C14 N3 . 1.468(3) ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
C15 N3 . 1.462(3) ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
N1 Re1 . 2.1624(17) ?
N2 Re1 . 2.2255(17) ?
Cl1 Re1 . 2.4885(7) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 Re1 . . 179.6(2) ?
O2 C2 Re1 . . 176.58(19) ?
O3 C3 Re1 . . 177.99(18) ?
N1 C4 C5 . . 122.4(2) ?
N1 C4 H4 . . 118.8 ?
C5 C4 H4 . . 118.8 ?
C4 C5 C6 . . 118.6(2) ?
C4 C5 H5 . . 120.7 ?
C6 C5 H5 . . 120.7 ?
C7 C6 C5 . . 119.56(19) ?
C7 C6 H6 . . 120.2 ?
C5 C6 H6 . . 120.2 ?
C6 C7 C8 . . 119.15(19) ?
C6 C7 H7 . . 120.4 ?
C8 C7 H7 . . 120.4 ?
N1 C8 C7 . . 120.82(19) ?
N1 C8 C9 . . 116.08(17) ?
C7 C8 C9 . . 123.03(18) ?
N2 C9 C10 . . 122.39(19) ?
N2 C9 C8 . . 115.07(17) ?
C10 C9 C8 . . 122.55(18) ?
C9 C10 C11 . . 118.57(19) ?
C9 C10 H10 . . 120.7 ?
C11 C10 H10 . . 120.7 ?
C12 C11 C10 . . 120.14(19) ?
C12 C11 H11 . . 119.9 ?
C10 C11 H11 . . 119.9 ?
C11 C12 C13 . . 119.24(19) ?
C11 C12 H12 . . 120.4 ?
C13 C12 H12 . . 120.4 ?
N2 C13 N3 . . 117.97(17) ?
N2 C13 C12 . . 120.48(18) ?
N3 C13 C12 . . 121.53(18) ?
N3 C14 H14A . . 109.5 ?
N3 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
N3 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
N3 C15 H15A . . 109.5 ?
N3 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
N3 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C8 N1 C4 . . 119.47(17) ?
C8 N1 Re1 . . 115.64(13) ?
C4 N1 Re1 . . 124.76(14) ?
C13 N2 C9 . . 118.60(17) ?
C13 N2 Re1 . . 126.43(13) ?
C9 N2 Re1 . . 111.50(13) ?
C13 N3 C15 . . 118.41(17) ?
C13 N3 C14 . . 119.60(17) ?
C15 N3 C14 . . 112.31(17) ?
C2 Re1 C1 . . 87.20(9) ?
C2 Re1 C3 . . 91.05(9) ?
C1 Re1 C3 . . 88.10(9) ?
C2 Re1 N1 . . 94.81(8) ?
C1 Re1 N1 . . 97.47(8) ?
C3 Re1 N1 . . 172.10(7) ?
C2 Re1 N2 . . 99.67(8) ?
C1 Re1 N2 . . 169.99(7) ?
C3 Re1 N2 . . 98.97(8) ?
N1 Re1 N2 . . 74.83(7) ?
C2 Re1 Cl1 . . 178.43(6) ?
C1 Re1 Cl1 . . 91.26(7) ?
C3 Re1 Cl1 . . 89.19(7) ?
N1 Re1 Cl1 . . 85.10(5) ?
N2 Re1 Cl1 . . 81.83(5) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C4 C5 C6 . . . . -1.1(3) ?
C4 C5 C6 C7 . . . . 1.6(3) ?
C5 C6 C7 C8 . . . . -0.2(3) ?
C6 C7 C8 N1 . . . . -1.7(3) ?
C6 C7 C8 C9 . . . . 175.11(18) ?
N1 C8 C9 N2 . . . . 12.2(2) ?
C7 C8 C9 N2 . . . . -164.74(17) ?
N1 C8 C9 C10 . . . . -168.42(18) ?
C7 C8 C9 C10 . . . . 14.6(3) ?
N2 C9 C10 C11 . . . . -0.4(3) ?
C8 C9 C10 C11 . . . . -179.77(19) ?
C9 C10 C11 C12 . . . . 3.7(3) ?
C10 C11 C12 C13 . . . . -0.7(3) ?
C11 C12 C13 N2 . . . . -5.9(3) ?
C11 C12 C13 N3 . . . . 175.76(19) ?
C7 C8 N1 C4 . . . . 2.3(3) ?
C9 C8 N1 C4 . . . . -174.76(17) ?
C7 C8 N1 Re1 . . . . -173.81(14) ?
C9 C8 N1 Re1 . . . . 9.2(2) ?
C5 C4 N1 C8 . . . . -0.9(3) ?
C5 C4 N1 Re1 . . . . 174.81(14) ?
N3 C13 N2 C9 . . . . -172.50(17) ?
C12 C13 N2 C9 . . . . 9.1(3) ?
N3 C13 N2 Re1 . . . . 30.4(2) ?
C12 C13 N2 Re1 . . . . -147.99(15) ?
C10 C9 N2 C13 . . . . -6.0(3) ?
C8 C9 N2 C13 . . . . 173.36(16) ?
C10 C9 N2 Re1 . . . . 154.33(16) ?
C8 C9 N2 Re1 . . . . -26.29(19) ?
N2 C13 N3 C15 . . . . -165.74(18) ?
C12 C13 N3 C15 . . . . 12.6(3) ?
N2 C13 N3 C14 . . . . 50.8(3) ?
C12 C13 N3 C14 . . . . -130.8(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_Ashley012918
_database_code_depnum_ccdc_archive 'CCDC 1908119'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2019-04-04 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C14 H11 Cl N3 O3 Re, C3 H7 N O'
_chemical_formula_sum            'C17 H18 Cl N4 O4 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         564.00

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   8.912(3)
_cell_length_b                   8.957(3)
_cell_length_c                   12.030(4)
_cell_angle_alpha                84.241(5)
_cell_angle_beta                 87.294(5)
_cell_angle_gamma                79.875(5)
_cell_volume                     940.1(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    120
_cell_measurement_theta_min      4.2978
_cell_measurement_theta_max      29.0918
_cell_measurement_temperature    103.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.089
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544

_exptl_absorpt_coefficient_mu    6.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.5729
_exptl_absorpt_correction_T_max  0.7461

_exptl_special_details           
;
;

_diffrn_ambient_temperature      103.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            23077
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             5677
_reflns_number_gt                5501
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0499
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_number_reflns         5677
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0150P)²+0.7497P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.492
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2016/6 (Bruker AXS, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  'SHELXTL XL 2016/6 (Bruker AXS, 2016)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4813(3) 0.8696(2) 0.62784(18) 0.0133(4) Uani d . . . 1 . .
C C2 0.5944(3) 0.8432(3) 0.8299(2) 0.0154(4) Uani d . . . 1 . .
C C3 0.7829(3) 0.8727(3) 0.6575(2) 0.0164(4) Uani d . . . 1 . .
C C4 0.4221(3) 0.5534(3) 0.8468(2) 0.0188(4) Uani d . . . 1 . .
H H4 0.394502 0.645075 0.881916 0.023 Uiso calc U . R 1 . .
C C5 0.3652(3) 0.4254(3) 0.8913(2) 0.0226(5) Uani d . . . 1 . .
H H5 0.301242 0.428439 0.956768 0.027 Uiso calc U . R 1 . .
C C6 0.4036(3) 0.2924(3) 0.8383(2) 0.0225(5) Uani d . . . 1 . .
H H6 0.36668 0.202735 0.867599 0.027 Uiso calc U . R 1 . .
C C7 0.4955(3) 0.2916(3) 0.7430(2) 0.0195(4) Uani d . . . 1 . .
H H7 0.520705 0.201781 0.705385 0.023 Uiso calc U . R 1 . .
C C8 0.5521(3) 0.4240(3) 0.70160(19) 0.0159(4) Uani d . . . 1 . .
C C9 0.6513(3) 0.4338(3) 0.60150(19) 0.0156(4) Uani d . . . 1 . .
C C10 0.6994(3) 0.3105(3) 0.5406(2) 0.0201(5) Uani d . . . 1 . .
H H10 0.667704 0.215645 0.562313 0.024 Uiso calc U . R 1 . .
C C11 0.7948(3) 0.3270(3) 0.4469(2) 0.0220(5) Uani d . . . 1 . .
H H11 0.832128 0.241798 0.406208 0.026 Uiso calc U . R 1 . .
C C12 0.8354(3) 0.4657(3) 0.4130(2) 0.0190(4) Uani d . . . 1 . .
H H12 0.900417 0.477828 0.349016 0.023 Uiso calc U . R 1 . .
C C13 0.7779(3) 0.5911(3) 0.47581(19) 0.0154(4) Uani d . . . 1 . .
C C14 0.8966(3) 0.7670(3) 0.3415(2) 0.0215(5) Uani d . . . 1 . .
H H14A 0.855093 0.732241 0.276553 0.032 Uiso calc U . R 1 . .
H H14B 1.002308 0.715561 0.351008 0.032 Uiso calc U . R 1 . .
H H14C 0.893397 0.877326 0.329889 0.032 Uiso calc U . R 1 . .
N N1 0.5163(2) 0.5524(2) 0.75448(17) 0.0156(4) Uani d . . . 1 . .
N N2 0.6938(2) 0.5727(2) 0.57177(16) 0.0141(4) Uani d . . . 1 . .
N N3 0.8054(2) 0.7308(2) 0.44156(17) 0.0185(4) Uani d . . . 1 . .
H H3 0.752(4) 0.802(4) 0.478(3) 0.022 Uiso d U . . 1 . .
Re Re1 0.64407(2) 0.73390(2) 0.70060(2) 0.01013(3) Uani d . . . 1 . .
O O1 0.3838(2) 0.9574(2) 0.58668(15) 0.0188(3) Uani d . . . 1 . .
O O2 0.5655(2) 0.9088(2) 0.90780(16) 0.0244(4) Uani d . . . 1 . .
O O3 0.8670(2) 0.9560(2) 0.63595(17) 0.0252(4) Uani d . . . 1 . .
Cl Cl1 0.85031(6) 0.55463(6) 0.80035(5) 0.01704(10) Uani d . . . 1 . .
C C15 -0.0503(3) 0.7709(3) 1.0243(2) 0.0232(5) Uani d . . . 1 . .
H H15A -0.11725 0.763629 0.963444 0.035 Uiso calc U . R 1 . .
H H15B -0.102058 0.846267 1.073296 0.035 Uiso calc U . R 1 . .
H H15C -0.026076 0.671415 1.067467 0.035 Uiso calc U . R 1 . .
C C16 0.2048(3) 0.8315(3) 1.0561(2) 0.0253(5) Uani d . . . 1 . .
H H16A 0.288084 0.874292 1.015886 0.038 Uiso calc U . R 1 . .
H H16B 0.245019 0.730656 1.092863 0.038 Uiso calc U . R 1 . .
H H16C 0.158785 0.898779 1.112443 0.038 Uiso calc U . R 1 . .
C C17 0.1121(3) 0.8490(3) 0.8677(2) 0.0259(5) Uani d . . . 1 . .
H H17 0.032697 0.837123 0.821075 0.031 Uiso calc U . R 1 . .
N N4 0.0903(2) 0.8176(3) 0.97770(18) 0.0205(4) Uani d . . . 1 . .
O O4 0.2232(3) 0.8911(3) 0.82153(19) 0.0392(6) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.158(3) ?
C1 Re1 . 1.906(2) ?
C2 O2 . 1.151(3) ?
C2 Re1 . 1.914(2) ?
C3 O3 . 1.151(3) ?
C3 Re1 . 1.923(2) ?
C4 N1 . 1.360(3) ?
C4 C5 . 1.383(3) ?
C4 H4 . 0.95 ?
C5 C6 . 1.390(4) ?
C5 H5 . 0.95 ?
C6 C7 . 1.377(4) ?
C6 H6 . 0.95 ?
C7 C8 . 1.406(3) ?
C7 H7 . 0.95 ?
C8 N1 . 1.352(3) ?
C8 C9 . 1.465(3) ?
C9 N2 . 1.373(3) ?
C9 C10 . 1.381(3) ?
C10 C11 . 1.391(4) ?
C10 H10 . 0.95 ?
C11 C12 . 1.373(4) ?
C11 H11 . 0.95 ?
C12 C13 . 1.423(3) ?
C12 H12 . 0.95 ?
C13 N3 . 1.338(3) ?
C13 N2 . 1.359(3) ?
C14 N3 . 1.461(3) ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
N1 Re1 . 2.175(2) ?
N2 Re1 . 2.200(2) ?
N3 H3 . 0.87(3) ?
Re1 Cl1 . 2.4861(8) ?
C15 N4 . 1.460(3) ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
C16 N4 . 1.451(3) ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 O4 . 1.212(3) ?
C17 N4 . 1.338(3) ?
C17 H17 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 Re1 . . 176.7(2) ?
O2 C2 Re1 . . 179.6(2) ?
O3 C3 Re1 . . 177.4(2) ?
N1 C4 C5 . . 122.3(2) ?
N1 C4 H4 . . 118.9 ?
C5 C4 H4 . . 118.9 ?
C4 C5 C6 . . 118.6(2) ?
C4 C5 H5 . . 120.7 ?
C6 C5 H5 . . 120.7 ?
C7 C6 C5 . . 119.5(2) ?
C7 C6 H6 . . 120.3 ?
C5 C6 H6 . . 120.3 ?
C6 C7 C8 . . 119.8(2) ?
C6 C7 H7 . . 120.1 ?
C8 C7 H7 . . 120.1 ?
N1 C8 C7 . . 120.4(2) ?
N1 C8 C9 . . 115.8(2) ?
C7 C8 C9 . . 123.8(2) ?
N2 C9 C10 . . 121.9(2) ?
N2 C9 C8 . . 116.1(2) ?
C10 C9 C8 . . 122.0(2) ?
C9 C10 C11 . . 119.1(2) ?
C9 C10 H10 . . 120.4 ?
C11 C10 H10 . . 120.4 ?
C12 C11 C10 . . 120.3(2) ?
C12 C11 H11 . . 119.8 ?
C10 C11 H11 . . 119.8 ?
C11 C12 C13 . . 118.5(2) ?
C11 C12 H12 . . 120.7 ?
C13 C12 H12 . . 120.7 ?
N3 C13 N2 . . 118.1(2) ?
N3 C13 C12 . . 120.7(2) ?
N2 C13 C12 . . 121.2(2) ?
N3 C14 H14A . . 109.5 ?
N3 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
N3 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C8 N1 C4 . . 119.3(2) ?
C8 N1 Re1 . . 116.36(16) ?
C4 N1 Re1 . . 123.54(16) ?
C13 N2 C9 . . 118.6(2) ?
C13 N2 Re1 . . 126.29(16) ?
C9 N2 Re1 . . 114.47(15) ?
C13 N3 C14 . . 124.2(2) ?
C13 N3 H3 . . 114.(2) ?
C14 N3 H3 . . 122.(2) ?
C1 Re1 C2 . . 87.77(10) ?
C1 Re1 C3 . . 91.10(10) ?
C2 Re1 C3 . . 86.51(10) ?
C1 Re1 N1 . . 96.87(9) ?
C2 Re1 N1 . . 96.02(9) ?
C3 Re1 N1 . . 171.71(8) ?
C1 Re1 N2 . . 97.57(9) ?
C2 Re1 N2 . . 169.81(9) ?
C3 Re1 N2 . . 101.99(9) ?
N1 Re1 N2 . . 74.79(8) ?
C1 Re1 Cl1 . . 178.13(7) ?
C2 Re1 Cl1 . . 91.21(7) ?
C3 Re1 Cl1 . . 90.39(7) ?
N1 Re1 Cl1 . . 81.68(6) ?
N2 Re1 Cl1 . . 83.20(5) ?
N4 C15 H15A . . 109.5 ?
N4 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
N4 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N4 C16 H16A . . 109.5 ?
N4 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
N4 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O4 C17 N4 . . 126.4(3) ?
O4 C17 H17 . . 116.8 ?
N4 C17 H17 . . 116.8 ?
C17 N4 C16 . . 121.2(2) ?
C17 N4 C15 . . 121.7(2) ?
C16 N4 C15 . . 117.1(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C4 C5 C6 . . . . -1.3(4) ?
C4 C5 C6 C7 . . . . -0.5(4) ?
C5 C6 C7 C8 . . . . 1.3(4) ?
C6 C7 C8 N1 . . . . -0.3(4) ?
C6 C7 C8 C9 . . . . 179.6(2) ?
N1 C8 C9 N2 . . . . -1.3(3) ?
C7 C8 C9 N2 . . . . 178.9(2) ?
N1 C8 C9 C10 . . . . 178.7(2) ?
C7 C8 C9 C10 . . . . -1.1(4) ?
N2 C9 C10 C11 . . . . 0.6(4) ?
C8 C9 C10 C11 . . . . -179.4(2) ?
C9 C10 C11 C12 . . . . -2.7(4) ?
C10 C11 C12 C13 . . . . 0.1(4) ?
C11 C12 C13 N3 . . . . -175.2(2) ?
C11 C12 C13 N2 . . . . 4.7(3) ?
C7 C8 N1 C4 . . . . -1.5(3) ?
C9 C8 N1 C4 . . . . 178.7(2) ?
C7 C8 N1 Re1 . . . . 168.90(17) ?
C9 C8 N1 Re1 . . . . -11.0(3) ?
C5 C4 N1 C8 . . . . 2.3(4) ?
C5 C4 N1 Re1 . . . . -167.37(19) ?
N3 C13 N2 C9 . . . . 173.2(2) ?
C12 C13 N2 C9 . . . . -6.7(3) ?
N3 C13 N2 Re1 . . . . -16.4(3) ?
C12 C13 N2 Re1 . . . . 163.68(17) ?
C10 C9 N2 C13 . . . . 4.0(3) ?
C8 C9 N2 C13 . . . . -175.97(19) ?
C10 C9 N2 Re1 . . . . -167.44(18) ?
C8 C9 N2 Re1 . . . . 12.6(2) ?
N2 C13 N3 C14 . . . . 178.7(2) ?
C12 C13 N3 C14 . . . . -1.4(4) ?
O4 C17 N4 C16 . . . . -0.3(5) ?
O4 C17 N4 C15 . . . . 178.6(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_Ashley_bisNMe2
_database_code_depnum_ccdc_archive 'CCDC 1908118'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2019-07-24 deposited with the CCDC.	2019-08-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            Ashley_bisNMe2
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H19 Cl4 N4 O3 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         667.39

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   9.368(5)
_cell_length_b                   11.275(6)
_cell_length_c                   11.587(6)
_cell_angle_alpha                75.978(9)
_cell_angle_beta                 76.488(8)
_cell_angle_gamma                81.595(8)
_cell_volume                     1149.3(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5513
_cell_measurement_theta_min      2.2526
_cell_measurement_theta_max      28.2059
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644

_exptl_absorpt_coefficient_mu    5.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_T_max  0.89

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            7978
_diffrn_reflns_av_R_equivalents  0.1633
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.949
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;

Refined as a 3-component twin.
;

_reflns_number_total             7978
_reflns_number_gt                5841
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.1016
_refine_ls_wR_factor_gt          0.2579
_refine_ls_wR_factor_ref         0.2963
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.013
_refine_ls_number_reflns         7978
_refine_ls_number_parameters     277
_refine_ls_number_restraints     261
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1896P)²+29.3759P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         11.085
_refine_diff_density_min         -6.164
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2018.7-1 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_publication_material  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.987(2) 0.5638(19) 0.1741(18) 0.016(3) Uani d . . . 1 . .
C C2 1.109(3) 0.592(2) 0.081(2) 0.027(5) Uani d . . . 1 . .
H H2 1.101506 0.654112 0.010362 0.033 Uiso calc U . R 1 . .
C C3 1.243(3) 0.525(2) 0.096(2) 0.026(4) Uani d . . . 1 . .
H H3 1.329586 0.543296 0.035695 0.032 Uiso calc U . R 1 . .
C C4 1.251(3) 0.435(3) 0.195(2) 0.032(5) Uani d . . . 1 . .
H H4 1.343898 0.391702 0.20572 0.038 Uiso calc U . R 1 . .
C C5 1.121(2) 0.4044(19) 0.2836(18) 0.015(3) Uani d U . . 1 . .
C C6 1.119(2) 0.2986(19) 0.3851(18) 0.015(3) Uani d U . . 1 . .
C C7 1.247(2) 0.221(2) 0.405(2) 0.022(4) Uani d . . . 1 . .
H H7 1.340995 0.240309 0.3566 0.027 Uiso calc U . R 1 . .
C C8 1.234(3) 0.118(2) 0.494(2) 0.026(5) Uani d . . . 1 . .
H H8 1.319196 0.062027 0.502423 0.032 Uiso calc U . R 1 . .
C C9 1.101(2) 0.093(2) 0.572(2) 0.021(4) Uani d . . . 1 . .
H H9 1.092991 0.020492 0.63495 0.025 Uiso calc U . R 1 . .
C C10 0.976(2) 0.1807(19) 0.5540(18) 0.015(3) Uani d U . . 1 . .
C C11 0.791(2) 0.701(2) 0.272(2) 0.025(5) Uani d . . . 1 . .
H H11A 0.817552 0.786024 0.245848 0.037 Uiso calc U . R 1 . .
H H11B 0.831411 0.660014 0.34401 0.037 Uiso calc U . R 1 . .
H H11C 0.683167 0.701834 0.292813 0.037 Uiso calc U . R 1 . .
C C12 0.829(3) 0.713(3) 0.053(2) 0.030(5) Uani d . . . 1 . .
H H12A 0.888303 0.783244 0.03174 0.045 Uiso calc U . R 1 . .
H H12B 0.724778 0.742887 0.059201 0.045 Uiso calc U . R 1 . .
H H12C 0.859959 0.664844 -0.009903 0.045 Uiso calc U . R 1 . .
C C13 0.782(3) 0.267(3) 0.696(2) 0.032(5) Uani d . . . 1 . .
H H13A 0.813952 0.344428 0.642228 0.048 Uiso calc U . R 1 . .
H H13B 0.814318 0.255571 0.772847 0.048 Uiso calc U . R 1 . .
H H13C 0.674034 0.270695 0.712069 0.048 Uiso calc U . R 1 . .
C C14 0.831(3) 0.046(2) 0.725(2) 0.029(5) Uani d . . . 1 . .
H H14A 0.852345 -0.019447 0.679998 0.044 Uiso calc U . R 1 . .
H H14B 0.729708 0.044243 0.773389 0.044 Uiso calc U . R 1 . .
H H14C 0.900068 0.034988 0.77923 0.044 Uiso calc U . R 1 . .
C C15 0.665(2) 0.437(2) 0.2679(19) 0.021(4) Uani d . . . 1 . .
C C16 0.7097(19) 0.4708(19) 0.4785(17) 0.016(3) Uani d U . . 1 . .
C C17 0.655(2) 0.255(2) 0.461(2) 0.025(4) Uani d . . . 1 . .
Cl Cl1 0.9140(5) 0.2242(5) 0.2321(4) 0.0199(9) Uani d . . . 1 . .
N N1 0.9915(19) 0.4679(16) 0.2696(15) 0.015(3) Uani d U . . 1 . .
N N2 0.9879(18) 0.2754(16) 0.4622(16) 0.015(3) Uani d U . . 1 . .
N N3 0.852(2) 0.6346(19) 0.1721(17) 0.024(4) Uani d . . . 1 . .
N N4 0.845(2) 0.1665(18) 0.6385(16) 0.020(3) Uani d . . . 1 . .
O O1 0.5851(18) 0.4804(18) 0.2044(15) 0.031(4) Uani d . . . 1 . .
O O2 0.6418(17) 0.5357(17) 0.5414(15) 0.029(3) Uani d . . . 1 . .
O O3 0.5670(19) 0.1843(18) 0.5117(16) 0.034(4) Uani d . . . 1 . .
Re Re1 0.79898(8) 0.36474(8) 0.37300(7) 0.0164(3) Uani d . . . 1 . .
C C18 0.345(3) -0.121(2) 0.860(2) 0.030(5) Uani d . . . 1 . .
H H18 0.301305 -0.178189 0.826414 0.036 Uiso calc U . R 1 . .
Cl Cl2 0.4313(7) -0.0123(7) 0.7387(6) 0.0395(15) Uani d . . . 1 . .
Cl Cl3 0.2033(8) -0.0501(7) 0.9566(6) 0.0435(16) Uani d . . . 1 . .
Cl Cl4 0.4778(10) -0.2072(8) 0.9428(8) 0.057(2) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.35(3) ?
C1 C2 . 1.39(3) ?
C1 N3 . 1.40(3) ?
C2 C3 . 1.39(4) ?
C2 H2 . 0.95 ?
C3 C4 . 1.34(4) ?
C3 H3 . 0.95 ?
C4 C5 . 1.42(3) ?
C4 H4 . 0.95 ?
C5 N1 . 1.34(3) ?
C5 C6 . 1.46(3) ?
C6 N2 . 1.36(3) ?
C6 C7 . 1.41(3) ?
C7 C8 . 1.35(3) ?
C7 H7 . 0.95 ?
C8 C9 . 1.38(3) ?
C8 H8 . 0.95 ?
C9 C10 . 1.44(3) ?
C9 H9 . 0.95 ?
C10 N2 . 1.31(3) ?
C10 N4 . 1.38(3) ?
C11 N3 . 1.49(3) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 N3 . 1.49(3) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 N4 . 1.44(3) ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 N4 . 1.48(3) ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
C15 O1 . 1.15(3) ?
C15 Re1 . 1.91(2) ?
C16 O2 . 1.17(2) ?
C16 Re1 . 1.888(18) ?
C17 O3 . 1.18(3) ?
C17 Re1 . 1.91(2) ?
Cl1 Re1 . 2.504(4) ?
N1 Re1 . 2.229(16) ?
N2 Re1 . 2.246(17) ?
C18 Cl2 . 1.75(2) ?
C18 Cl3 . 1.76(2) ?
C18 Cl4 . 1.78(3) ?
C18 H18 . 1.0 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 . . 123.(2) ?
N1 C1 N3 . . 116.5(17) ?
C2 C1 N3 . . 121.(2) ?
C3 C2 C1 . . 117.(2) ?
C3 C2 H2 . . 121.5 ?
C1 C2 H2 . . 121.5 ?
C4 C3 C2 . . 121.(2) ?
C4 C3 H3 . . 119.6 ?
C2 C3 H3 . . 119.6 ?
C3 C4 C5 . . 120.(2) ?
C3 C4 H4 . . 120.0 ?
C5 C4 H4 . . 120.0 ?
N1 C5 C4 . . 120.(2) ?
N1 C5 C6 . . 117.1(18) ?
C4 C5 C6 . . 123.(2) ?
N2 C6 C7 . . 119.7(18) ?
N2 C6 C5 . . 118.0(19) ?
C7 C6 C5 . . 122.3(19) ?
C8 C7 C6 . . 119.(2) ?
C8 C7 H7 . . 120.5 ?
C6 C7 H7 . . 120.5 ?
C7 C8 C9 . . 122.(2) ?
C7 C8 H8 . . 119.1 ?
C9 C8 H8 . . 119.1 ?
C8 C9 C10 . . 117.(2) ?
C8 C9 H9 . . 121.6 ?
C10 C9 H9 . . 121.6 ?
N2 C10 N4 . . 121.(2) ?
N2 C10 C9 . . 120.5(18) ?
N4 C10 C9 . . 118.8(18) ?
N3 C11 H11A . . 109.5 ?
N3 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
N3 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
N3 C12 H12A . . 109.5 ?
N3 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N3 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N4 C13 H13A . . 109.5 ?
N4 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
N4 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
N4 C14 H14A . . 109.5 ?
N4 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
N4 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
O1 C15 Re1 . . 180.(2) ?
O2 C16 Re1 . . 173.6(16) ?
O3 C17 Re1 . . 177.(2) ?
C5 N1 C1 . . 119.3(16) ?
C5 N1 Re1 . . 113.0(12) ?
C1 N1 Re1 . . 124.6(13) ?
C10 N2 C6 . . 121.8(18) ?
C10 N2 Re1 . . 123.0(13) ?
C6 N2 Re1 . . 110.9(13) ?
C1 N3 C12 . . 117.4(18) ?
C1 N3 C11 . . 117.9(18) ?
C12 N3 C11 . . 110.6(19) ?
C10 N4 C13 . . 117.8(18) ?
C10 N4 C14 . . 117.3(19) ?
C13 N4 C14 . . 112.0(19) ?
C16 Re1 C17 . . 87.4(10) ?
C16 Re1 C15 . . 90.2(9) ?
C17 Re1 C15 . . 87.5(9) ?
C16 Re1 N1 . . 99.1(7) ?
C17 Re1 N1 . . 171.4(9) ?
C15 Re1 N1 . . 98.1(8) ?
C16 Re1 N2 . . 99.3(7) ?
C17 Re1 N2 . . 99.0(8) ?
C15 Re1 N2 . . 168.7(7) ?
N1 Re1 N2 . . 74.5(6) ?
C16 Re1 Cl1 . . 179.2(6) ?
C17 Re1 Cl1 . . 92.2(8) ?
C15 Re1 Cl1 . . 89.1(7) ?
N1 Re1 Cl1 . . 81.4(5) ?
N2 Re1 Cl1 . . 81.5(5) ?
Cl2 C18 Cl3 . . 111.0(14) ?
Cl2 C18 Cl4 . . 109.4(13) ?
Cl3 C18 Cl4 . . 109.8(13) ?
Cl2 C18 H18 . . 108.9 ?
Cl3 C18 H18 . . 108.9 ?
Cl4 C18 H18 . . 108.9 ?


# start Validation Reply Form
_vrf_PLAT029_Ashley_bisNMe2      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.949 Why?  
RESPONSE: The specimen was a low quality crystal containing three domains.
Several different crystals were tried and this specimen produced the best
structure. The obtained result is only used to establish the connectivity
of the sample. No further information is derived from the structure.
;
_vrf_PLAT097_Ashley_bisNMe2      
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      11.09 eA-3  
RESPONSE: The specimen was a low quality crystal containing three domains.
Several different crystals were tried and this specimen produced the best
structure. The obtained result is only used to establish the connectivity
of the sample. No further information is derived from the structure.
;
_vrf_PLAT342_Ashley_bisNMe2      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03111 Ang.  
RESPONSE: The specimen was a low quality crystal containing three domains.
Several different crystals were tried and this specimen produced the best
structure. The obtained result is only used to establish the connectivity
of the sample. No further information is derived from the structure.
;
# end Validation Reply Form
