# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_60min_405nm
_database_code_depnum_ccdc_archive 'CCDC 1842772'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.6151(5)
_cell_length_b                   22.6151(5)
_cell_length_c                   6.5646(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3357.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2343
_cell_measurement_theta_min      3.2260
_cell_measurement_theta_max      27.6020

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0105
-1 1 0 0.0135
1 -1 0 0.0135
1 1 0 0.0164
-1 1 1 0.1144
1 -1 -1 0.1144
_exptl_absorpt_coefficient_mu    7.283
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6059
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.848
_diffrn_reflns_theta_max         25.667
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.929
_reflns_number_total             2928
_reflns_number_gt                2529
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_max     0.835
_reflns_Friedel_fraction_full    0.846

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)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 863 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2928
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0793
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4464(6) 0.3591(6) 0.147(3) 0.032(3) Uani 1 1 d . U . . .
C2 C 0.3996(7) 0.3229(7) 0.498(2) 0.033(3) Uani 1 1 d . U . . .
C3 C 0.5092(7) 0.3674(7) 0.493(2) 0.033(3) Uani 1 1 d . U . . .
C4 C 0.4859(7) 0.2172(7) 0.715(2) 0.033(3) Uani 1 1 d . U . . .
H4 H 0.4540 0.2389 0.7724 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5056(6) 0.1679(6) 0.823(2) 0.032(3) Uani 1 1 d . U . . .
H5 H 0.4866 0.1552 0.9441 0.038 Uiso 1 1 calc R U . . .
C6 C 0.5545(7) 0.1383(7) 0.743(2) 0.033(3) Uani 1 1 d . U . . .
C7 C 0.5784(7) 0.1581(7) 0.563(2) 0.028(3) Uani 1 1 d . U . . .
H7 H 0.6115 0.1380 0.5063 0.034 Uiso 1 1 calc R U . . .
C8 C 0.5554(7) 0.2063(6) 0.464(2) 0.028(3) Uani 1 1 d . U . . .
C9 C 0.5798(7) 0.2293(7) 0.271(2) 0.026(3) Uani 1 1 d . U . . .
C10 C 0.6274(6) 0.2060(6) 0.173(2) 0.027(3) Uani 1 1 d . U . . .
H10 H 0.6465 0.1723 0.2290 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6485(7) 0.2304(7) -0.004(2) 0.028(3) Uani 1 1 d . U . . .
C12 C 0.6186(6) 0.2798(7) -0.082(2) 0.029(3) Uani 1 1 d . U . . .
H12 H 0.6314 0.2985 -0.2039 0.035 Uiso 1 1 calc R U . . .
C13 C 0.5707(7) 0.2999(7) 0.022(2) 0.036(4) Uani 1 1 d . U . . .
H13 H 0.5507 0.3335 -0.0313 0.044 Uiso 1 1 calc R U . . .
C14 C 0.5538(8) 0.0701(7) 1.016(2) 0.040(4) Uani 1 1 d . U . . .
H14A H 0.5115 0.0627 0.9961 0.059 Uiso 1 1 calc R U . . .
H14B H 0.5591 0.0999 1.1227 0.059 Uiso 1 1 calc R U . . .
H14C H 0.5735 0.0334 1.0562 0.059 Uiso 1 1 calc R U . . .
C15 C 0.7200(7) 0.2320(8) -0.272(2) 0.038(4) Uani 1 1 d . U . . .
H15A H 0.6892 0.2355 -0.3765 0.057 Uiso 1 1 calc R U . . .
H15B H 0.7523 0.2074 -0.3242 0.057 Uiso 1 1 calc R U . . .
H15C H 0.7351 0.2713 -0.2383 0.057 Uiso 1 1 calc R U . . .
N2 N 0.5074(6) 0.2369(6) 0.5382(19) 0.033(2) Uani 1 1 d . U . . .
N3 N 0.5499(5) 0.2768(5) 0.1901(19) 0.030(2) Uani 1 1 d . U . . .
O3 O 0.4343(5) 0.3914(5) 0.0132(17) 0.050(3) Uani 1 1 d . U . . .
O4 O 0.3565(5) 0.3353(5) 0.5800(16) 0.042(3) Uani 1 1 d . U . . .
O5 O 0.5315(5) 0.4058(5) 0.5794(18) 0.054(3) Uani 1 1 d . U . . .
O6 O 0.5790(5) 0.0912(4) 0.8296(17) 0.042(3) Uani 1 1 d . U . . .
O7 O 0.6954(4) 0.2050(5) -0.0922(13) 0.034(2) Uani 1 1 d . U . . .
Re1 Re 0.47094(3) 0.30540(3) 0.34988(9) 0.02828(18) Uani 1 1 d . U . . .
N1 N 0.4222(15) 0.2262(9) 0.198(6) 0.037(2) Uani 0.457(14) 1 d D U P A 1
O1 O 0.4377(10) 0.1768(9) 0.238(3) 0.037(2) Uani 0.457(14) 1 d D U P A 1
O2 O 0.3822(11) 0.2368(10) 0.089(4) 0.037(2) Uani 0.457(14) 1 d D U P A 1
N1A N 0.3922(10) 0.2179(8) 0.114(4) 0.037(2) Uani 0.543(14) 1 d D U P A 2
O1A O 0.4407(8) 0.2279(8) 0.213(4) 0.037(2) Uani 0.543(14) 1 d D U P A 2
O2A O 0.3634(8) 0.2669(8) 0.095(3) 0.037(2) Uani 0.543(14) 1 d D U P A 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
C1 O3 1.173(17) . ?
C1 Re1 1.887(16) . ?
C2 O4 1.151(17) . ?
C2 Re1 1.923(16) . ?
C3 O5 1.155(17) . ?
C3 Re1 1.895(16) . ?
C4 N2 1.333(17) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.40(2) . ?
C5 H5 0.9500 . ?
C6 O6 1.327(18) . ?
C6 C7 1.37(2) . ?
C7 C8 1.37(2) . ?
C7 H7 0.9500 . ?
C8 N2 1.376(18) . ?
C8 C9 1.479(19) . ?
C9 C10 1.358(19) . ?
C9 N3 1.375(18) . ?
C10 C11 1.37(2) . ?
C10 H10 0.9500 . ?
C11 O7 1.337(17) . ?
C11 C12 1.40(2) . ?
C12 C13 1.36(2) . ?
C12 H12 0.9500 . ?
C13 N3 1.31(2) . ?
C13 H13 0.9500 . ?
C14 O6 1.430(17) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.441(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.146(13) . ?
N3 Re1 2.171(12) . ?
Re1 O1A 2.09(2) . ?
Re1 N1 2.33(3) . ?
N1 O2 1.18(3) . ?
N1 O1 1.200(10) . ?
N1A O2A 1.290(13) . ?
N1A O1A 1.293(13) . ?

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
O3 C1 Re1 175.7(13) . . ?
O4 C2 Re1 177.0(15) . . ?
O5 C3 Re1 178.7(15) . . ?
N2 C4 C5 126.3(15) . . ?
N2 C4 H4 116.8 . . ?
C5 C4 H4 116.8 . . ?
C4 C5 C6 116.5(14) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
O6 C6 C7 117.8(15) . . ?
O6 C6 C5 123.6(14) . . ?
C7 C6 C5 118.6(15) . . ?
C6 C7 C8 121.1(15) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 N2 122.1(14) . . ?
C7 C8 C9 122.9(14) . . ?
N2 C8 C9 115.0(13) . . ?
C10 C9 N3 120.7(13) . . ?
C10 C9 C8 124.4(14) . . ?
N3 C9 C8 114.9(13) . . ?
C9 C10 C11 121.3(14) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
O7 C11 C10 118.0(14) . . ?
O7 C11 C12 124.4(13) . . ?
C10 C11 C12 117.5(14) . . ?
C13 C12 C11 117.8(14) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
N3 C13 C12 125.1(15) . . ?
N3 C13 H13 117.4 . . ?
C12 C13 H13 117.4 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 115.3(13) . . ?
C4 N2 Re1 127.0(11) . . ?
C8 N2 Re1 117.5(10) . . ?
C13 N3 C9 117.5(14) . . ?
C13 N3 Re1 125.7(11) . . ?
C9 N3 Re1 116.8(9) . . ?
C6 O6 C14 118.0(12) . . ?
C11 O7 C15 118.6(12) . . ?
C1 Re1 C3 90.4(7) . . ?
C1 Re1 C2 88.7(7) . . ?
C3 Re1 C2 88.9(6) . . ?
C1 Re1 O1A 98.0(7) . . ?
C3 Re1 O1A 170.0(7) . . ?
C2 Re1 O1A 96.6(8) . . ?
C1 Re1 N2 169.8(6) . . ?
C3 Re1 N2 94.2(6) . . ?
C2 Re1 N2 100.3(6) . . ?
O1A Re1 N2 76.6(6) . . ?
C1 Re1 N3 95.3(6) . . ?
C3 Re1 N3 94.8(6) . . ?
C2 Re1 N3 174.5(6) . . ?
O1A Re1 N3 79.1(7) . . ?
N2 Re1 N3 75.4(5) . . ?
C1 Re1 N1 93.0(8) . . ?
C3 Re1 N1 175.7(11) . . ?
C2 Re1 N1 88.7(11) . . ?
N2 Re1 N1 82.7(7) . . ?
N3 Re1 N1 87.3(9) . . ?
O2 N1 O1 123(3) . . ?
O2 N1 Re1 117.9(16) . . ?
O1 N1 Re1 119(2) . . ?
O2A N1A O1A 109.0(13) . . ?
N1A O1A Re1 129.9(12) . . ?

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
N2 C4 C5 C6 4(2) . . . . ?
C4 C5 C6 O6 179.0(14) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
O6 C6 C7 C8 179.7(14) . . . . ?
C5 C6 C7 C8 1(2) . . . . ?
C6 C7 C8 N2 0(2) . . . . ?
C6 C7 C8 C9 179.8(14) . . . . ?
C7 C8 C9 C10 -1(2) . . . . ?
N2 C8 C9 C10 179.2(14) . . . . ?
C7 C8 C9 N3 178.0(14) . . . . ?
N2 C8 C9 N3 -1.8(19) . . . . ?
N3 C9 C10 C11 2(2) . . . . ?
C8 C9 C10 C11 -178.7(14) . . . . ?
C9 C10 C11 O7 -179.6(13) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
O7 C11 C12 C13 178.5(14) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 N3 0(2) . . . . ?
C5 C4 N2 C8 -3(2) . . . . ?
C5 C4 N2 Re1 171.3(11) . . . . ?
C7 C8 N2 C4 1(2) . . . . ?
C9 C8 N2 C4 -178.7(13) . . . . ?
C7 C8 N2 Re1 -173.6(12) . . . . ?
C9 C8 N2 Re1 6.3(17) . . . . ?
C12 C13 N3 C9 2(2) . . . . ?
C12 C13 N3 Re1 -176.6(12) . . . . ?
C10 C9 N3 C13 -3(2) . . . . ?
C8 C9 N3 C13 178.1(13) . . . . ?
C10 C9 N3 Re1 175.7(11) . . . . ?
C8 C9 N3 Re1 -3.4(16) . . . . ?
C7 C6 O6 C14 -179.4(14) . . . . ?
C5 C6 O6 C14 0(2) . . . . ?
C10 C11 O7 C15 -176.6(13) . . . . ?
C12 C11 O7 C15 5(2) . . . . ?
O2A N1A O1A Re1 5(4) . . . . ?

_refine_diff_density_max         1.198
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.150


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_GS_150K
_database_code_depnum_ccdc_archive 'CCDC 1842773'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.2989(5)
_cell_length_b                   22.2989(5)
_cell_length_c                   6.6471(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3305.21(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3857
_cell_measurement_theta_min      3.6520
_cell_measurement_theta_max      29.1570

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.024
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0144
1 -1 0 0.0096
0 0 -1 0.1568
0 0 1 0.1728
-1 0 0 0.0206
1 0 0 0.0135
0 -1 0 0.0283
0 1 0 0.0230
_exptl_absorpt_coefficient_mu    7.398
_exptl_absorpt_correction_T_min  0.459
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6711
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.889
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3356
_reflns_number_gt                3171
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_max     0.973
_reflns_Friedel_fraction_full    0.986

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)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 1345 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3356
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3612(4) 0.5589(3) 0.8685(13) 0.0232(17) Uani 1 1 d . U . . .
C2 C 0.3263(4) 0.6060(4) 0.5136(13) 0.0194(16) Uani 1 1 d . U . . .
C3 C 0.3695(4) 0.4940(4) 0.5206(14) 0.0244(17) Uani 1 1 d . U . . .
C4 C 0.2169(4) 0.5226(4) 0.2990(12) 0.0207(16) Uani 1 1 d . U . . .
H4 H 0.2372 0.5571 0.2498 0.025 Uiso 1 1 calc R U . . .
C5 C 0.1697(3) 0.5012(4) 0.1904(13) 0.0204(15) Uani 1 1 d . U . . .
H5 H 0.1578 0.5200 0.0685 0.024 Uiso 1 1 calc R U . . .
C6 C 0.1394(4) 0.4510(4) 0.2631(12) 0.0199(16) Uani 1 1 d . U . . .
C7 C 0.1585(4) 0.4246(4) 0.4408(12) 0.0214(17) Uani 1 1 d . U . . .
H7 H 0.1385 0.3904 0.4931 0.026 Uiso 1 1 calc R U . . .
C8 C 0.2069(3) 0.4489(3) 0.5405(11) 0.0146(13) Uani 1 1 d . U . . .
C9 C 0.2288(3) 0.4242(3) 0.7349(12) 0.0138(13) Uani 1 1 d . U . . .
C10 C 0.2056(3) 0.3741(3) 0.8231(12) 0.0173(14) Uani 1 1 d . U . . .
H10 H 0.1732 0.3534 0.7614 0.021 Uiso 1 1 calc R U . . .
C11 C 0.2297(3) 0.3531(3) 1.0057(12) 0.0167(14) Uani 1 1 d . U . . .
C12 C 0.2777(4) 0.3840(4) 1.0864(12) 0.0187(15) Uani 1 1 d . U . . .
H12 H 0.2961 0.3705 1.2070 0.022 Uiso 1 1 calc R U . . .
C13 C 0.2984(4) 0.4344(3) 0.9909(13) 0.0195(16) Uani 1 1 d . U . . .
H13 H 0.3308 0.4556 1.0506 0.023 Uiso 1 1 calc R U . . .
C14 C 0.0712(4) 0.4512(4) -0.0137(13) 0.030(2) Uani 1 1 d . U . . .
H14A H 0.0604 0.4934 0.0071 0.045 Uiso 1 1 calc R U . . .
H14B H 0.0360 0.4290 -0.0607 0.045 Uiso 1 1 calc R U . . .
H14C H 0.1031 0.4486 -0.1147 0.045 Uiso 1 1 calc R U . . .
C15 C 0.2313(4) 0.2788(4) 1.2618(12) 0.0246(19) Uani 1 1 d . U . . .
H15A H 0.2346 0.3099 1.3655 0.037 Uiso 1 1 calc R U . . .
H15B H 0.2714 0.2636 1.2287 0.037 Uiso 1 1 calc R U . . .
H15C H 0.2064 0.2459 1.3120 0.037 Uiso 1 1 calc R U . . .
N1 N 0.2294(3) 0.5810(3) 0.8053(10) 0.0193(13) Uani 1 1 d . U . . .
N2 N 0.2368(3) 0.4979(3) 0.4728(10) 0.0163(12) Uani 1 1 d . U . . .
N3 N 0.2756(3) 0.4554(3) 0.8175(11) 0.0152(12) Uani 1 1 d . U . . .
O1 O 0.1765(3) 0.5650(3) 0.7677(9) 0.0307(14) Uani 1 1 d . U . . .
O2 O 0.2372(3) 0.6218(3) 0.9229(9) 0.0341(15) Uani 1 1 d . U . . .
O3 O 0.3928(3) 0.5704(3) 0.9981(11) 0.0445(18) Uani 1 1 d . U . . .
O4 O 0.3393(3) 0.6493(3) 0.4283(9) 0.0304(15) Uani 1 1 d . U . . .
O5 O 0.4060(3) 0.4699(3) 0.4318(11) 0.0444(19) Uani 1 1 d . U . . .
O6 O 0.0917(3) 0.4263(3) 0.1705(10) 0.0288(13) Uani 1 1 d . U . . .
O7 O 0.2042(3) 0.3040(3) 1.0840(8) 0.0212(12) Uani 1 1 d . U . . .
Re1 Re 0.30591(2) 0.53499(2) 0.66110(4) 0.01640(10) Uani 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 O3 1.143(10) . ?
C1 Re1 1.925(8) . ?
C2 O4 1.156(10) . ?
C2 Re1 1.917(8) . ?
C3 O5 1.140(10) . ?
C3 Re1 1.928(9) . ?
C4 N2 1.355(10) . ?
C4 C5 1.362(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(11) . ?
C5 H5 0.9500 . ?
C6 O6 1.348(10) . ?
C6 C7 1.386(11) . ?
C7 C8 1.376(11) . ?
C7 H7 0.9500 . ?
C8 N2 1.357(9) . ?
C8 C9 1.488(11) . ?
C9 C10 1.363(10) . ?
C9 N3 1.370(10) . ?
C10 C11 1.407(11) . ?
C10 H10 0.9500 . ?
C11 O7 1.340(9) . ?
C11 C12 1.380(11) . ?
C12 C13 1.371(11) . ?
C12 H12 0.9500 . ?
C13 N3 1.344(12) . ?
C13 H13 0.9500 . ?
C14 O6 1.420(11) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.441(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1 O2 1.212(9) . ?
N1 O1 1.260(9) . ?
N1 Re1 2.209(7) . ?
N2 Re1 2.151(6) . ?
N3 Re1 2.165(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
O3 C1 Re1 176.1(7) . . ?
O4 C2 Re1 178.5(8) . . ?
O5 C3 Re1 177.8(8) . . ?
N2 C4 C5 124.2(8) . . ?
N2 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C4 C5 C6 118.1(8) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
O6 C6 C7 117.3(8) . . ?
O6 C6 C5 123.6(7) . . ?
C7 C6 C5 119.1(8) . . ?
C8 C7 C6 119.0(8) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
N2 C8 C7 122.8(7) . . ?
N2 C8 C9 115.1(7) . . ?
C7 C8 C9 122.0(7) . . ?
C10 C9 N3 122.2(7) . . ?
C10 C9 C8 123.5(7) . . ?
N3 C9 C8 114.2(7) . . ?
C9 C10 C11 119.9(7) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
O7 C11 C12 125.8(7) . . ?
O7 C11 C10 116.4(7) . . ?
C12 C11 C10 117.8(7) . . ?
C13 C12 C11 119.3(7) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
N3 C13 C12 123.8(8) . . ?
N3 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 118.3(7) . . ?
O2 N1 Re1 121.3(5) . . ?
O1 N1 Re1 120.4(5) . . ?
C4 N2 C8 116.7(7) . . ?
C4 N2 Re1 125.0(5) . . ?
C8 N2 Re1 118.0(5) . . ?
C13 N3 C9 117.0(7) . . ?
C13 N3 Re1 125.4(6) . . ?
C9 N3 Re1 117.5(5) . . ?
C6 O6 C14 119.2(7) . . ?
C11 O7 C15 117.3(7) . . ?
C2 Re1 C1 89.2(4) . . ?
C2 Re1 C3 88.3(3) . . ?
C1 Re1 C3 90.5(4) . . ?
C2 Re1 N2 101.0(3) . . ?
C1 Re1 N2 169.2(3) . . ?
C3 Re1 N2 93.6(3) . . ?
C2 Re1 N3 175.3(3) . . ?
C1 Re1 N3 94.8(3) . . ?
C3 Re1 N3 94.2(3) . . ?
N2 Re1 N3 75.0(2) . . ?
C2 Re1 N1 91.2(3) . . ?
C1 Re1 N1 93.1(3) . . ?
C3 Re1 N1 176.4(3) . . ?
N2 Re1 N1 83.0(3) . . ?
N3 Re1 N1 86.1(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 0.7(12) . . . . ?
C4 C5 C6 O6 179.0(8) . . . . ?
C4 C5 C6 C7 -0.4(12) . . . . ?
O6 C6 C7 C8 -179.5(8) . . . . ?
C5 C6 C7 C8 0.0(12) . . . . ?
C6 C7 C8 N2 0.3(12) . . . . ?
C6 C7 C8 C9 178.2(7) . . . . ?
N2 C8 C9 C10 -177.8(7) . . . . ?
C7 C8 C9 C10 4.1(12) . . . . ?
N2 C8 C9 N3 0.8(9) . . . . ?
C7 C8 C9 N3 -177.2(7) . . . . ?
N3 C9 C10 C11 0.3(12) . . . . ?
C8 C9 C10 C11 178.9(7) . . . . ?
C9 C10 C11 O7 179.4(7) . . . . ?
C9 C10 C11 C12 -1.6(11) . . . . ?
O7 C11 C12 C13 -178.9(7) . . . . ?
C10 C11 C12 C13 2.2(11) . . . . ?
C11 C12 C13 N3 -1.6(13) . . . . ?
C5 C4 N2 C8 -0.4(12) . . . . ?
C5 C4 N2 Re1 -174.3(6) . . . . ?
C7 C8 N2 C4 -0.1(11) . . . . ?
C9 C8 N2 C4 -178.1(6) . . . . ?
C7 C8 N2 Re1 174.3(6) . . . . ?
C9 C8 N2 Re1 -3.8(8) . . . . ?
C12 C13 N3 C9 0.3(12) . . . . ?
C12 C13 N3 Re1 179.4(6) . . . . ?
C10 C9 N3 C13 0.3(11) . . . . ?
C8 C9 N3 C13 -178.3(7) . . . . ?
C10 C9 N3 Re1 -178.9(6) . . . . ?
C8 C9 N3 Re1 2.5(8) . . . . ?
C7 C6 O6 C14 -179.0(7) . . . . ?
C5 C6 O6 C14 1.5(12) . . . . ?
C12 C11 O7 C15 -4.0(11) . . . . ?
C10 C11 O7 C15 174.9(7) . . . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.106


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_5min_405nm
_database_code_depnum_ccdc_archive 'CCDC 1842775'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT342_5min_405nm          
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03 Ang.
RESPONSE: Weak high angle data due to unavoidable crystal damage following 
irradiation. 
Contributing to lower data to parameter ratio and slightly reducing precision 
on C-C bonds.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.5083(8)
_cell_length_b                   22.5083(8)
_cell_length_c                   6.5855(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3336.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1874
_cell_measurement_theta_min      3.2210
_cell_measurement_theta_max      26.6370

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0105
-1 1 0 0.0135
1 -1 0 0.0135
-1 -1 0 0.0164
-1 1 -1 0.1144
1 -1 1 0.1144
_exptl_absorpt_coefficient_mu    7.329
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6083
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.862
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.931
_reflns_number_total             2918
_reflns_number_gt                2438
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_max     0.835
_reflns_Friedel_fraction_full    0.849

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)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 730 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2918
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4456(8) 0.1410(8) -0.106(3) 0.032(3) Uani 1 1 d . U . . .
C2 C 0.3976(9) 0.1756(9) 0.244(3) 0.031(3) Uani 1 1 d . U . . .
C3 C 0.5085(9) 0.1311(9) 0.240(3) 0.030(3) Uani 1 1 d . U . . .
C4 C 0.4839(9) 0.2826(8) 0.461(3) 0.030(4) Uani 1 1 d . U . . .
H4 H 0.4522 0.2605 0.5190 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5028(8) 0.3320(8) 0.569(3) 0.030(4) Uani 1 1 d . U . . .
H5 H 0.4831 0.3451 0.6885 0.036 Uiso 1 1 calc R U . . .
C6 C 0.5513(8) 0.3607(8) 0.493(3) 0.024(4) Uani 1 1 d . U . . .
C7 C 0.5766(8) 0.3418(8) 0.310(3) 0.025(4) Uani 1 1 d . U . . .
H7 H 0.6090 0.3629 0.2523 0.030 Uiso 1 1 calc R U . . .
C8 C 0.5543(8) 0.2929(8) 0.214(3) 0.026(4) Uani 1 1 d . U . . .
C9 C 0.5796(8) 0.2707(8) 0.019(3) 0.024(3) Uani 1 1 d . U . . .
C10 C 0.6265(7) 0.2932(8) -0.078(3) 0.026(3) Uani 1 1 d . U . . .
H10 H 0.6464 0.3264 -0.0200 0.031 Uiso 1 1 calc R U . . .
C11 C 0.6470(8) 0.2706(8) -0.258(3) 0.022(3) Uani 1 1 d . U . . .
C12 C 0.6192(9) 0.2211(9) -0.331(3) 0.032(4) Uani 1 1 d . U . . .
H12 H 0.6341 0.2011 -0.4472 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5687(8) 0.2003(9) -0.232(3) 0.030(4) Uani 1 1 d . U . . .
H13 H 0.5481 0.1674 -0.2890 0.035 Uiso 1 1 calc R U . . .
C14 C 0.5529(9) 0.4283(9) 0.767(3) 0.042(5) Uani 1 1 d . U . . .
H14A H 0.5098 0.4330 0.7538 0.063 Uiso 1 1 calc R U . . .
H14B H 0.5707 0.4665 0.8038 0.063 Uiso 1 1 calc R U . . .
H14C H 0.5615 0.3991 0.8739 0.063 Uiso 1 1 calc R U . . .
C15 C 0.7209(9) 0.2688(9) -0.519(3) 0.033(5) Uani 1 1 d . U . . .
H15A H 0.6890 0.2603 -0.6161 0.049 Uiso 1 1 calc R U . . .
H15B H 0.7411 0.2317 -0.4830 0.049 Uiso 1 1 calc R U . . .
H15C H 0.7494 0.2963 -0.5808 0.049 Uiso 1 1 calc R U . . .
N2 N 0.5055(7) 0.2625(7) 0.284(2) 0.027(2) Uani 1 1 d . U . . .
N3 N 0.5483(7) 0.2236(7) -0.065(2) 0.027(2) Uani 1 1 d . U . . .
O3 O 0.4325(7) 0.1081(7) -0.239(2) 0.052(4) Uani 1 1 d . U . . .
O4 O 0.3553(6) 0.1634(6) 0.329(2) 0.041(4) Uani 1 1 d . U . . .
O5 O 0.5309(7) 0.0943(7) 0.329(2) 0.055(5) Uani 1 1 d . U . . .
O6 O 0.5769(6) 0.4084(6) 0.581(2) 0.044(4) Uani 1 1 d . U . . .
O7 O 0.6963(5) 0.2951(5) -0.3405(16) 0.028(3) Uani 1 1 d . U . . .
Re1 Re 0.46915(3) 0.19444(3) 0.09658(11) 0.0267(2) Uani 1 1 d . U . . .
N1 N 0.4203(12) 0.2734(9) -0.052(5) 0.034(2) Uani 0.581(17) 1 d D U P A 1
O1 O 0.4375(9) 0.3228(9) -0.018(3) 0.034(2) Uani 0.581(17) 1 d D U P A 1
O2 O 0.3796(11) 0.2629(9) -0.162(4) 0.034(2) Uani 0.581(17) 1 d D U P A 1
N1A N 0.3935(16) 0.2808(12) -0.150(6) 0.034(2) Uani 0.419(17) 1 d D U P A 2
O1A O 0.4400(13) 0.2712(13) -0.039(6) 0.034(2) Uani 0.419(17) 1 d D U P A 2
O2A O 0.3645(12) 0.2311(13) -0.166(4) 0.034(2) Uani 0.419(17) 1 d D U P A 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
C1 O3 1.18(2) . ?
C1 Re1 1.87(2) . ?
C2 O4 1.14(2) . ?
C2 Re1 1.93(2) . ?
C3 O5 1.13(2) . ?
C3 Re1 1.926(19) . ?
C4 N2 1.34(2) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.37(2) . ?
C5 H5 0.9500 . ?
C6 O6 1.35(2) . ?
C6 C7 1.40(2) . ?
C7 C8 1.37(2) . ?
C7 H7 0.9500 . ?
C8 N2 1.37(2) . ?
C8 C9 1.49(2) . ?
C9 C10 1.34(2) . ?
C9 N3 1.39(2) . ?
C10 C11 1.37(2) . ?
C10 H10 0.9500 . ?
C11 O7 1.35(2) . ?
C11 C12 1.37(2) . ?
C12 C13 1.39(2) . ?
C12 H12 0.9500 . ?
C13 N3 1.30(2) . ?
C13 H13 0.9500 . ?
C14 O6 1.41(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.429(18) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.129(15) . ?
N3 Re1 2.174(15) . ?
Re1 O1A 2.05(3) . ?
Re1 N1 2.31(2) . ?
N1 O2 1.191(13) . ?
N1 O1 1.198(13) . ?
N1A O1A 1.295(13) . ?
N1A O2A 1.299(13) . ?

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
O3 C1 Re1 177.5(17) . . ?
O4 C2 Re1 178.6(18) . . ?
O5 C3 Re1 178.0(18) . . ?
N2 C4 C5 127.3(18) . . ?
N2 C4 H4 116.4 . . ?
C5 C4 H4 116.4 . . ?
C6 C5 C4 115.8(18) . . ?
C6 C5 H5 122.1 . . ?
C4 C5 H5 122.1 . . ?
O6 C6 C5 123.8(17) . . ?
O6 C6 C7 116.2(17) . . ?
C5 C6 C7 119.9(18) . . ?
C8 C7 C6 119.7(18) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 N2 122.7(17) . . ?
C7 C8 C9 121.9(17) . . ?
N2 C8 C9 115.4(16) . . ?
C10 C9 N3 120.1(16) . . ?
C10 C9 C8 126.0(18) . . ?
N3 C9 C8 113.9(16) . . ?
C9 C10 C11 122.7(17) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 H10 118.6 . . ?
O7 C11 C12 124.5(16) . . ?
O7 C11 C10 118.3(16) . . ?
C12 C11 C10 116.9(17) . . ?
C11 C12 C13 119.0(17) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
N3 C13 C12 123.3(19) . . ?
N3 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 114.4(16) . . ?
C4 N2 Re1 127.4(13) . . ?
C8 N2 Re1 118.1(12) . . ?
C13 N3 C9 117.7(17) . . ?
C13 N3 Re1 125.5(14) . . ?
C9 N3 Re1 116.9(12) . . ?
C6 O6 C14 117.7(14) . . ?
C11 O7 C15 118.7(14) . . ?
C1 Re1 C3 90.2(9) . . ?
C1 Re1 C2 89.0(8) . . ?
C3 Re1 C2 88.5(8) . . ?
C1 Re1 O1A 98.0(10) . . ?
C3 Re1 O1A 169.6(9) . . ?
C2 Re1 O1A 97.9(11) . . ?
C1 Re1 N2 169.4(7) . . ?
C3 Re1 N2 94.1(7) . . ?
C2 Re1 N2 100.8(7) . . ?
O1A Re1 N2 76.7(9) . . ?
C1 Re1 N3 94.4(7) . . ?
C3 Re1 N3 95.0(7) . . ?
C2 Re1 N3 175.1(7) . . ?
O1A Re1 N3 78.2(11) . . ?
N2 Re1 N3 75.6(6) . . ?
C1 Re1 N1 93.3(8) . . ?
C3 Re1 N1 175.8(10) . . ?
C2 Re1 N1 89.2(10) . . ?
N2 Re1 N1 82.8(7) . . ?
N3 Re1 N1 87.1(9) . . ?
O2 N1 O1 123.3(19) . . ?
O2 N1 Re1 118.0(16) . . ?
O1 N1 Re1 118.7(15) . . ?
O1A N1A O2A 107.9(15) . . ?
N1A O1A Re1 130.1(17) . . ?

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
N2 C4 C5 C6 -5(3) . . . . ?
C4 C5 C6 O6 -177.9(17) . . . . ?
C4 C5 C6 C7 4(3) . . . . ?
O6 C6 C7 C8 178.2(17) . . . . ?
C5 C6 C7 C8 -3(3) . . . . ?
C6 C7 C8 N2 3(3) . . . . ?
C6 C7 C8 C9 -179.7(16) . . . . ?
C7 C8 C9 C10 3(3) . . . . ?
N2 C8 C9 C10 179.7(18) . . . . ?
C7 C8 C9 N3 -174.9(18) . . . . ?
N2 C8 C9 N3 2(2) . . . . ?
N3 C9 C10 C11 -2(3) . . . . ?
C8 C9 C10 C11 -179.6(17) . . . . ?
C9 C10 C11 O7 -177.5(16) . . . . ?
C9 C10 C11 C12 -3(3) . . . . ?
O7 C11 C12 C13 -179.9(17) . . . . ?
C10 C11 C12 C13 6(3) . . . . ?
C11 C12 C13 N3 -4(3) . . . . ?
C5 C4 N2 C8 5(3) . . . . ?
C5 C4 N2 Re1 -170.5(15) . . . . ?
C7 C8 N2 C4 -4(3) . . . . ?
C9 C8 N2 C4 179.0(15) . . . . ?
C7 C8 N2 Re1 171.8(14) . . . . ?
C9 C8 N2 Re1 -5(2) . . . . ?
C12 C13 N3 C9 -1(3) . . . . ?
C12 C13 N3 Re1 179.1(14) . . . . ?
C10 C9 N3 C13 4(3) . . . . ?
C8 C9 N3 C13 -177.8(16) . . . . ?
C10 C9 N3 Re1 -175.9(14) . . . . ?
C8 C9 N3 Re1 1.8(19) . . . . ?
C5 C6 O6 C14 2(3) . . . . ?
C7 C6 O6 C14 -179.3(16) . . . . ?
C12 C11 O7 C15 1(3) . . . . ?
C10 C11 O7 C15 175.0(15) . . . . ?
O2A N1A O1A Re1 0(6) . . . . ?

_refine_diff_density_max         1.000
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.185


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_180min_405nm
_database_code_depnum_ccdc_archive 'CCDC 1842776'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT973_180min_405nm        
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 1.88 eA-3
RESPONSE: Slightly weak high angle data and so loss of resolution, due
to the extended period crystal irradiation. Reduced data resolution 
likely leads to truncation errors and spurious peaks in the region of the 
heavy atom.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.6482(5)
_cell_length_b                   22.6482(5)
_cell_length_c                   6.5591(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3364.42(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5776
_cell_measurement_theta_min      3.5890
_cell_measurement_theta_max      29.0660

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.102
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0116
-1 -1 0 0.0116
1 -1 -1 0.1206
-1 1 1 0.1391
1 -1 0 0.0096
-1 1 0 0.0096
_exptl_absorpt_coefficient_mu    7.268
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            11493
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.844
_diffrn_reflns_theta_max         25.636
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3157
_reflns_number_gt                2939
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0564P)²+20.4266P] 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 1192 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.048(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3157
_refine_ls_number_parameters     235
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.1083
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.5540(7) 0.6399(7) 0.645(3) 0.034(3) Uani 1 1 d . U . . .
C2 C 0.5995(7) 0.6766(7) 0.998(2) 0.030(3) Uani 1 1 d . U . . .
C3 C 0.4902(7) 0.6297(7) 0.990(3) 0.035(3) Uani 1 1 d . U . . .
C4 C 0.5156(7) 0.7832(7) 1.214(2) 0.031(3) Uani 1 1 d . U . . .
H4 H 0.5490 0.7630 1.2660 0.038 Uiso 1 1 calc R U . . .
C5 C 0.4939(7) 0.8313(7) 1.321(2) 0.030(3) Uani 1 1 d . U . . .
H5 H 0.5122 0.8437 1.4437 0.036 Uiso 1 1 calc R U . . .
C6 C 0.4451(7) 0.8611(7) 1.245(3) 0.031(3) Uani 1 1 d . U . . .
C7 C 0.4206(8) 0.8414(7) 1.063(2) 0.030(3) Uani 1 1 d . U . . .
H7 H 0.3872 0.8609 1.0070 0.036 Uiso 1 1 calc R U . . .
C8 C 0.4448(7) 0.7936(7) 0.964(2) 0.027(3) Uani 1 1 d . U . . .
C9 C 0.4204(7) 0.7706(7) 0.770(2) 0.029(3) Uani 1 1 d . U . . .
C10 C 0.3714(6) 0.7937(7) 0.674(2) 0.028(3) Uani 1 1 d . U . . .
H10 H 0.3510 0.8263 0.7318 0.033 Uiso 1 1 calc R U . . .
C11 C 0.3520(7) 0.7694(7) 0.493(2) 0.029(3) Uani 1 1 d . U . . .
C12 C 0.3789(7) 0.7192(8) 0.418(2) 0.035(3) Uani 1 1 d . U . . .
H12 H 0.3639 0.6991 0.3022 0.042 Uiso 1 1 calc R U . . .
C13 C 0.4290(7) 0.6990(8) 0.521(2) 0.032(3) Uani 1 1 d . U . . .
H13 H 0.4499 0.6665 0.4645 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4458(10) 0.9304(9) 1.515(3) 0.050(5) Uani 1 1 d . U . . .
H14A H 0.4882 0.9372 1.4973 0.075 Uiso 1 1 calc R U . . .
H14B H 0.4396 0.9010 1.6226 0.075 Uiso 1 1 calc R U . . .
H14C H 0.4265 0.9675 1.5541 0.075 Uiso 1 1 calc R U . . .
C15 C 0.2801(8) 0.7693(8) 0.224(3) 0.040(4) Uani 1 1 d . U . . .
H15A H 0.3103 0.7690 0.1172 0.060 Uiso 1 1 calc R U . . .
H15B H 0.2462 0.7927 0.1787 0.060 Uiso 1 1 calc R U . . .
H15C H 0.2674 0.7288 0.2528 0.060 Uiso 1 1 calc R U . . .
N2 N 0.4916(6) 0.7641(6) 1.040(2) 0.029(2) Uani 1 1 d . U . . .
N3 N 0.4490(6) 0.7227(6) 0.6915(19) 0.028(2) Uani 1 1 d . U . . .
O3 O 0.5662(6) 0.6084(6) 0.514(2) 0.052(3) Uani 1 1 d . U . . .
O4 O 0.6436(5) 0.6649(5) 1.0802(18) 0.041(3) Uani 1 1 d . U . . .
O5 O 0.4681(6) 0.5937(6) 1.082(2) 0.056(4) Uani 1 1 d . U . . .
O6 O 0.4209(5) 0.9093(5) 1.3277(18) 0.043(3) Uani 1 1 d . U . . .
O7 O 0.3044(5) 0.7953(5) 0.4075(15) 0.037(3) Uani 1 1 d . U . . .
Re1 Re 0.52878(3) 0.69454(3) 0.84999(9) 0.0278(2) Uani 1 1 d . U . . .
N1 N 0.5770(12) 0.7745(10) 0.691(4) 0.036(2) Uani 0.420(16) 1 d D U P A 1
O1 O 0.5616(11) 0.8228(10) 0.741(4) 0.036(2) Uani 0.420(16) 1 d D U P A 1
O2 O 0.6181(12) 0.7644(11) 0.584(4) 0.036(2) Uani 0.420(16) 1 d D U P A 1
N1A N 0.6065(9) 0.7817(8) 0.616(4) 0.036(2) Uani 0.580(16) 1 d D U P A 2
O1A O 0.5586(7) 0.7717(9) 0.714(3) 0.036(2) Uani 0.580(16) 1 d D U P A 2
O2A O 0.6356(8) 0.7329(8) 0.596(3) 0.036(2) Uani 0.580(16) 1 d D U P A 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
C1 O3 1.15(2) . ?
C1 Re1 1.916(17) . ?
C2 O4 1.164(18) . ?
C2 Re1 1.918(16) . ?
C3 O5 1.13(2) . ?
C3 Re1 1.941(17) . ?
C4 N2 1.33(2) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(2) . ?
C5 H5 0.9500 . ?
C6 O6 1.34(2) . ?
C6 C7 1.39(2) . ?
C7 C8 1.38(2) . ?
C7 H7 0.9500 . ?
C8 N2 1.349(19) . ?
C8 C9 1.48(2) . ?
C9 N3 1.37(2) . ?
C9 C10 1.38(2) . ?
C10 C11 1.38(2) . ?
C10 H10 0.9500 . ?
C11 O7 1.347(18) . ?
C11 C12 1.38(2) . ?
C12 C13 1.40(2) . ?
C12 H12 0.9500 . ?
C13 N3 1.32(2) . ?
C13 H13 0.9500 . ?
C14 O6 1.44(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.447(19) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.180(13) . ?
N3 Re1 2.180(13) . ?
Re1 O1A 2.075(19) . ?
Re1 N1 2.36(2) . ?
N1 O2 1.188(14) . ?
N1 O1 1.195(14) . ?
N1A O1A 1.281(13) . ?
N1A O2A 1.294(13) . ?

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
O3 C1 Re1 175.6(15) . . ?
O4 C2 Re1 177.0(14) . . ?
O5 C3 Re1 176.0(16) . . ?
N2 C4 C5 122.8(15) . . ?
N2 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C6 C5 C4 119.0(15) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
O6 C6 C5 125.3(15) . . ?
O6 C6 C7 116.6(15) . . ?
C5 C6 C7 118.0(16) . . ?
C8 C7 C6 119.9(15) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
N2 C8 C7 121.8(15) . . ?
N2 C8 C9 116.1(13) . . ?
C7 C8 C9 122.2(14) . . ?
N3 C9 C10 120.6(15) . . ?
N3 C9 C8 115.2(13) . . ?
C10 C9 C8 124.1(15) . . ?
C9 C10 C11 119.9(15) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
O7 C11 C12 124.4(14) . . ?
O7 C11 C10 115.9(14) . . ?
C12 C11 C10 119.5(15) . . ?
C11 C12 C13 117.3(15) . . ?
C11 C12 H12 121.3 . . ?
C13 C12 H12 121.3 . . ?
N3 C13 C12 123.6(16) . . ?
N3 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 118.5(14) . . ?
C4 N2 Re1 124.4(11) . . ?
C8 N2 Re1 116.6(10) . . ?
C13 N3 C9 118.7(14) . . ?
C13 N3 Re1 124.7(11) . . ?
C9 N3 Re1 116.5(10) . . ?
C6 O6 C14 117.4(13) . . ?
C11 O7 C15 118.2(13) . . ?
C1 Re1 C2 88.3(7) . . ?
C1 Re1 C3 88.8(7) . . ?
C2 Re1 C3 88.6(7) . . ?
C1 Re1 O1A 98.4(7) . . ?
C2 Re1 O1A 97.2(7) . . ?
C3 Re1 O1A 170.9(7) . . ?
C1 Re1 N3 95.8(6) . . ?
C2 Re1 N3 175.1(6) . . ?
C3 Re1 N3 94.3(6) . . ?
O1A Re1 N3 79.5(6) . . ?
C1 Re1 N2 170.0(6) . . ?
C2 Re1 N2 100.7(6) . . ?
C3 Re1 N2 95.8(6) . . ?
O1A Re1 N2 76.3(6) . . ?
N3 Re1 N2 75.0(5) . . ?
C1 Re1 N1 92.7(8) . . ?
C2 Re1 N1 90.0(8) . . ?
C3 Re1 N1 177.9(9) . . ?
N3 Re1 N1 87.0(8) . . ?
N2 Re1 N1 82.9(7) . . ?
O2 N1 O1 124(2) . . ?
O2 N1 Re1 118.5(18) . . ?
O1 N1 Re1 116.6(17) . . ?
O1A N1A O2A 109.6(14) . . ?
N1A O1A Re1 129.7(13) . . ?

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
N2 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 O6 -177.3(15) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
O6 C6 C7 C8 177.0(15) . . . . ?
C5 C6 C7 C8 0(2) . . . . ?
C6 C7 C8 N2 1(2) . . . . ?
C6 C7 C8 C9 179.8(15) . . . . ?
N2 C8 C9 N3 -0.8(19) . . . . ?
C7 C8 C9 N3 -179.5(15) . . . . ?
N2 C8 C9 C10 177.5(15) . . . . ?
C7 C8 C9 C10 -1(2) . . . . ?
N3 C9 C10 C11 -2(2) . . . . ?
C8 C9 C10 C11 179.8(14) . . . . ?
C9 C10 C11 O7 -179.0(14) . . . . ?
C9 C10 C11 C12 5(2) . . . . ?
O7 C11 C12 C13 177.9(14) . . . . ?
C10 C11 C12 C13 -7(2) . . . . ?
C11 C12 C13 N3 5(2) . . . . ?
C5 C4 N2 C8 1(2) . . . . ?
C5 C4 N2 Re1 173.6(11) . . . . ?
C7 C8 N2 C4 -2(2) . . . . ?
C9 C8 N2 C4 179.4(14) . . . . ?
C7 C8 N2 Re1 -174.8(12) . . . . ?
C9 C8 N2 Re1 6.5(16) . . . . ?
C12 C13 N3 C9 -2(2) . . . . ?
C12 C13 N3 Re1 -177.7(12) . . . . ?
C10 C9 N3 C13 0(2) . . . . ?
C8 C9 N3 C13 178.7(13) . . . . ?
C10 C9 N3 Re1 176.4(11) . . . . ?
C8 C9 N3 Re1 -5.3(17) . . . . ?
C5 C6 O6 C14 -3(2) . . . . ?
C7 C6 O6 C14 -179.8(16) . . . . ?
C12 C11 O7 C15 -1(2) . . . . ?
C10 C11 O7 C15 -176.3(14) . . . . ?
O2A N1A O1A Re1 5(3) . . . . ?

_refine_diff_density_max         2.502
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.195


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_15min_405nm
_database_code_depnum_ccdc_archive 'CCDC 1842779'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.5635(5)
_cell_length_b                   22.5635(5)
_cell_length_c                   6.5794(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3349.65(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2514
_cell_measurement_theta_min      3.6050
_cell_measurement_theta_max      27.6000

_exptl_crystal_description       needles
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0105
1 -1 0 0.0135
-1 1 0 0.0135
1 1 0 0.0164
1 -1 -1 0.1144
-1 1 1 0.1144
_exptl_absorpt_coefficient_mu    7.300
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6080
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.855
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.930
_reflns_number_total             2928
_reflns_number_gt                2605
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_max     0.838
_reflns_Friedel_fraction_full    0.849

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)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 916 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.038(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2928
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6403(6) 0.5545(6) 0.856(3) 0.033(3) Uani 1 1 d . U . . .
C2 C 0.6768(6) 0.6007(7) 0.506(2) 0.029(3) Uani 1 1 d . U . . .
C3 C 0.6323(7) 0.4914(7) 0.510(2) 0.033(3) Uani 1 1 d . U . . .
C4 C 0.7826(7) 0.5156(7) 0.289(2) 0.032(3) Uani 1 1 d . U . . .
H4 H 0.7613 0.5482 0.2337 0.039 Uiso 1 1 calc R U . . .
C5 C 0.8310(6) 0.4963(6) 0.180(2) 0.031(3) Uani 1 1 d . U . . .
H5 H 0.8432 0.5154 0.0582 0.037 Uiso 1 1 calc R U . . .
C6 C 0.8615(6) 0.4469(7) 0.257(2) 0.031(3) Uani 1 1 d . U . . .
C7 C 0.8423(6) 0.4222(6) 0.438(2) 0.026(3) Uani 1 1 d . U . . .
H7 H 0.8628 0.3895 0.4954 0.031 Uiso 1 1 calc R U . . .
C8 C 0.7935(6) 0.4452(6) 0.534(2) 0.026(3) Uani 1 1 d . U . . .
C9 C 0.7712(6) 0.4209(6) 0.729(2) 0.025(3) Uani 1 1 d . U . . .
C10 C 0.7940(6) 0.3730(6) 0.825(2) 0.025(3) Uani 1 1 d . U . . .
H10 H 0.8273 0.3533 0.7682 0.030 Uiso 1 1 calc R U . . .
C11 C 0.7699(6) 0.3524(6) 1.0039(19) 0.022(2) Uani 1 1 d . U . . .
C12 C 0.7202(6) 0.3816(6) 1.083(2) 0.030(3) Uani 1 1 d . U . . .
H12 H 0.7013 0.3679 1.2035 0.036 Uiso 1 1 calc R U . . .
C13 C 0.6999(7) 0.4309(6) 0.982(2) 0.034(3) Uani 1 1 d . U . . .
H13 H 0.6671 0.4518 1.0370 0.040 Uiso 1 1 calc R U . . .
C14 C 0.9296(7) 0.4464(7) -0.019(2) 0.045(4) Uani 1 1 d . U . . .
H14A H 0.8984 0.4430 -0.1218 0.068 Uiso 1 1 calc R U . . .
H14B H 0.9648 0.4245 -0.0634 0.068 Uiso 1 1 calc R U . . .
H14C H 0.9398 0.4882 0.0006 0.068 Uiso 1 1 calc R U . . .
C15 C 0.7688(7) 0.2795(7) 1.272(2) 0.034(4) Uani 1 1 d . U . . .
H15A H 0.7302 0.2623 1.2369 0.050 Uiso 1 1 calc R U . . .
H15B H 0.7633 0.3108 1.3734 0.050 Uiso 1 1 calc R U . . .
H15C H 0.7946 0.2486 1.3269 0.050 Uiso 1 1 calc R U . . .
N2 N 0.7626(5) 0.4935(5) 0.4631(18) 0.030(2) Uani 1 1 d . U . . .
N3 N 0.7238(5) 0.4508(5) 0.8091(18) 0.029(2) Uani 1 1 d . U . . .
O3 O 0.6081(5) 0.5668(5) 0.9875(16) 0.048(3) Uani 1 1 d . U . . .
O4 O 0.6642(5) 0.6441(4) 0.4223(16) 0.041(3) Uani 1 1 d . U . . .
O5 O 0.5939(5) 0.4687(5) 0.4208(18) 0.056(3) Uani 1 1 d . U . . .
O6 O 0.9086(4) 0.4220(5) 0.1708(17) 0.042(3) Uani 1 1 d . U . . .
O7 O 0.7955(4) 0.3044(4) 1.0914(12) 0.031(2) Uani 1 1 d . U . . .
Re1 Re 0.69451(2) 0.53005(2) 0.65197(8) 0.02694(17) Uani 1 1 d . U . . .
N1 N 0.7733(8) 0.5786(11) 0.805(5) 0.0359(19) Uani 0.524(13) 1 d D U P A 1
O1 O 0.8231(7) 0.5630(8) 0.765(3) 0.0359(19) Uani 0.524(13) 1 d D U P A 1
O2 O 0.7634(8) 0.6196(9) 0.914(3) 0.0359(19) Uani 0.524(13) 1 d D U P A 1
N1A N 0.7817(8) 0.6078(11) 0.889(5) 0.0359(19) Uani 0.476(13) 1 d D U P A 2
O1A O 0.7723(9) 0.5601(9) 0.786(4) 0.0359(19) Uani 0.476(13) 1 d D U P A 2
O2A O 0.7325(8) 0.6363(8) 0.910(3) 0.0359(19) Uani 0.476(13) 1 d D U P A 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
C1 O3 1.164(17) . ?
C1 Re1 1.898(15) . ?
C2 O4 1.158(16) . ?
C2 Re1 1.905(15) . ?
C3 O5 1.164(17) . ?
C3 Re1 1.899(15) . ?
C4 N2 1.329(17) . ?
C4 C5 1.377(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.404(19) . ?
C5 H5 0.9500 . ?
C6 O6 1.331(17) . ?
C6 C7 1.383(19) . ?
C7 C8 1.372(19) . ?
C7 H7 0.9500 . ?
C8 N2 1.373(17) . ?
C8 C9 1.481(18) . ?
C9 C10 1.354(18) . ?
C9 N3 1.371(18) . ?
C10 C11 1.377(18) . ?
C10 H10 0.9500 . ?
C11 O7 1.354(15) . ?
C11 C12 1.402(19) . ?
C12 C13 1.379(19) . ?
C12 H12 0.9500 . ?
C13 N3 1.334(19) . ?
C13 H13 0.9500 . ?
C14 O6 1.443(17) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.444(14) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.142(12) . ?
N3 Re1 2.169(12) . ?
Re1 O1A 2.08(2) . ?
Re1 N1 2.318(19) . ?
N1 O2 1.191(12) . ?
N1 O1 1.207(13) . ?
N1A O1A 1.289(13) . ?
N1A O2A 1.290(13) . ?

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
O3 C1 Re1 176.2(13) . . ?
O4 C2 Re1 177.2(13) . . ?
O5 C3 Re1 178.6(14) . . ?
N2 C4 C5 126.7(14) . . ?
N2 C4 H4 116.6 . . ?
C5 C4 H4 116.6 . . ?
C4 C5 C6 116.8(14) . . ?
C4 C5 H5 121.6 . . ?
C6 C5 H5 121.6 . . ?
O6 C6 C7 116.5(13) . . ?
O6 C6 C5 124.9(13) . . ?
C7 C6 C5 118.6(14) . . ?
C8 C7 C6 119.7(14) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 N2 123.3(13) . . ?
C7 C8 C9 122.0(13) . . ?
N2 C8 C9 114.6(12) . . ?
C10 C9 N3 120.5(12) . . ?
C10 C9 C8 124.9(13) . . ?
N3 C9 C8 114.6(12) . . ?
C9 C10 C11 121.4(13) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
O7 C11 C10 117.7(12) . . ?
O7 C11 C12 123.9(12) . . ?
C10 C11 C12 118.4(13) . . ?
C13 C12 C11 117.7(13) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
N3 C13 C12 123.4(14) . . ?
N3 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 114.8(13) . . ?
C4 N2 Re1 126.8(10) . . ?
C8 N2 Re1 118.1(9) . . ?
C13 N3 C9 118.6(13) . . ?
C13 N3 Re1 124.0(11) . . ?
C9 N3 Re1 117.3(9) . . ?
C6 O6 C14 118.0(11) . . ?
C11 O7 C15 118.8(11) . . ?
C1 Re1 C3 90.3(7) . . ?
C1 Re1 C2 88.8(6) . . ?
C3 Re1 C2 88.9(6) . . ?
C1 Re1 O1A 98.6(7) . . ?
C3 Re1 O1A 169.5(7) . . ?
C2 Re1 O1A 96.8(8) . . ?
C1 Re1 N2 170.0(5) . . ?
C3 Re1 N2 93.9(5) . . ?
C2 Re1 N2 100.4(5) . . ?
O1A Re1 N2 76.4(7) . . ?
C1 Re1 N3 95.7(5) . . ?
C3 Re1 N3 94.6(5) . . ?
C2 Re1 N3 174.3(6) . . ?
O1A Re1 N3 79.0(8) . . ?
N2 Re1 N3 75.0(4) . . ?
C1 Re1 N1 92.8(7) . . ?
C3 Re1 N1 176.2(9) . . ?
C2 Re1 N1 89.1(9) . . ?
N2 Re1 N1 83.3(6) . . ?
N3 Re1 N1 87.1(8) . . ?
O2 N1 O1 122.2(17) . . ?
O2 N1 Re1 119.0(14) . . ?
O1 N1 Re1 118.7(14) . . ?
O1A N1A O2A 109.3(14) . . ?
N1A O1A Re1 129.4(13) . . ?

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
N2 C4 C5 C6 2(2) . . . . ?
C4 C5 C6 O6 179.2(14) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
O6 C6 C7 C8 -179.1(13) . . . . ?
C5 C6 C7 C8 2(2) . . . . ?
C6 C7 C8 N2 -2(2) . . . . ?
C6 C7 C8 C9 -179.6(13) . . . . ?
C7 C8 C9 C10 -3(2) . . . . ?
N2 C8 C9 C10 178.9(14) . . . . ?
C7 C8 C9 N3 177.0(14) . . . . ?
N2 C8 C9 N3 -0.9(18) . . . . ?
N3 C9 C10 C11 1(2) . . . . ?
C8 C9 C10 C11 -178.7(12) . . . . ?
C9 C10 C11 O7 -179.7(12) . . . . ?
C9 C10 C11 C12 1(2) . . . . ?
O7 C11 C12 C13 178.2(13) . . . . ?
C10 C11 C12 C13 -3(2) . . . . ?
C11 C12 C13 N3 2(2) . . . . ?
C5 C4 N2 C8 -2(2) . . . . ?
C5 C4 N2 Re1 171.6(11) . . . . ?
C7 C8 N2 C4 2(2) . . . . ?
C9 C8 N2 C4 179.8(12) . . . . ?
C7 C8 N2 Re1 -172.3(11) . . . . ?
C9 C8 N2 Re1 5.5(16) . . . . ?
C12 C13 N3 C9 0(2) . . . . ?
C12 C13 N3 Re1 -177.7(11) . . . . ?
C10 C9 N3 C13 -2(2) . . . . ?
C8 C9 N3 C13 178.2(12) . . . . ?
C10 C9 N3 Re1 176.2(10) . . . . ?
C8 C9 N3 Re1 -4.0(15) . . . . ?
C7 C6 O6 C14 179.6(13) . . . . ?
C5 C6 O6 C14 -1(2) . . . . ?
C10 C11 O7 C15 -176.0(12) . . . . ?
C12 C11 O7 C15 3.3(19) . . . . ?
O2A N1A O1A Re1 3(4) . . . . ?

_refine_diff_density_max         0.999
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.149


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_150K
_database_code_depnum_ccdc_archive 'CCDC 1842777'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.7194(19)
_cell_length_b                   22.7194(19)
_cell_length_c                   6.5611(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3386.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2750
_cell_measurement_theta_min      3.5670
_cell_measurement_theta_max      30.6310

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
-1 -1 -1 0.1206
1 1 1 0.1391
-1 1 0 0.0116
1 1 0 0.0096
-1 -1 0 0.0096
_exptl_absorpt_coefficient_mu    7.220
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6030
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.232
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.935
_reflns_number_total             2903
_reflns_number_gt                2587
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_max     0.857
_reflns_Friedel_fraction_full    0.860

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0391P)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 925 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2903
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.005
_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
C1 C 0.4009(7) 0.8236(7) 0.252(2) 0.023(3) Uani 1 1 d . U . . .
C2 C 0.4458(7) 0.8596(7) 0.607(3) 0.029(3) Uani 1 1 d . U . . .
C3 C 0.5091(7) 0.8689(7) 0.256(2) 0.023(3) Uani 1 1 d . U . . .
C4 C 0.5718(7) 0.8018(7) 0.734(2) 0.025(3) Uani 1 1 d . U . . .
H4 H 0.5526 0.8345 0.7880 0.030 Uiso 1 1 calc R U . . .
C5 C 0.6204(7) 0.7805(7) 0.832(2) 0.022(3) Uani 1 1 d . U . . .
H5 H 0.6344 0.7993 0.9483 0.027 Uiso 1 1 calc R U . . .
C6 C 0.6484(7) 0.7312(7) 0.759(2) 0.024(3) Uani 1 1 d . U . . .
C7 C 0.6282(6) 0.7062(7) 0.575(2) 0.022(3) Uani 1 1 d . U . . .
H7 H 0.6470 0.6734 0.5209 0.027 Uiso 1 1 calc R U . . .
C8 C 0.5803(7) 0.7307(7) 0.477(2) 0.022(3) Uani 1 1 d . U . . .
C9 C 0.5556(7) 0.7054(7) 0.286(2) 0.022(3) Uani 1 1 d . U . . .
C10 C 0.5797(7) 0.6589(7) 0.188(2) 0.025(3) Uani 1 1 d . U . . .
H10 H 0.6132 0.6408 0.2399 0.030 Uiso 1 1 calc R U . . .
C11 C 0.5545(7) 0.6384(7) 0.009(2) 0.023(3) Uani 1 1 d . U . . .
C12 C 0.5062(7) 0.6693(7) -0.073(2) 0.027(3) Uani 1 1 d . U . . .
H12 H 0.4889 0.6578 -0.1951 0.032 Uiso 1 1 calc R U . . .
C13 C 0.4858(7) 0.7172(7) 0.035(2) 0.026(3) Uani 1 1 d . U . . .
H13 H 0.4537 0.7377 -0.0170 0.031 Uiso 1 1 calc R U . . .
C14 C 0.7194(8) 0.7312(9) 1.026(2) 0.037(4) Uani 1 1 d . U . . .
H14A H 0.7330 0.7702 0.9943 0.055 Uiso 1 1 calc R U . . .
H14B H 0.7518 0.7081 1.0757 0.055 Uiso 1 1 calc R U . . .
H14C H 0.6893 0.7333 1.1280 0.055 Uiso 1 1 calc R U . . .
C15 C 0.5535(9) 0.5700(9) -0.265(3) 0.044(5) Uani 1 1 d . U . . .
H15A H 0.5611 0.5976 -0.3726 0.065 Uiso 1 1 calc R U . . .
H15B H 0.5118 0.5657 -0.2468 0.065 Uiso 1 1 calc R U . . .
H15C H 0.5704 0.5325 -0.2996 0.065 Uiso 1 1 calc R U . . .
N2 N 0.5501(6) 0.7772(6) 0.5583(18) 0.021(2) Uani 1 1 d . U . . .
N3 N 0.5095(6) 0.7359(6) 0.2099(19) 0.0220(19) Uani 1 1 d . U . . .
O3 O 0.3567(5) 0.8347(5) 0.1674(17) 0.036(3) Uani 1 1 d . U . . .
O4 O 0.4337(6) 0.8914(6) 0.7354(19) 0.048(4) Uani 1 1 d . U . . .
O5 O 0.5319(6) 0.9057(6) 0.1688(19) 0.046(4) Uani 1 1 d . U . . .
O6 O 0.6958(5) 0.7042(5) 0.8440(14) 0.032(3) Uani 1 1 d . U . . .
O7 O 0.5792(5) 0.5908(5) -0.0813(18) 0.039(3) Uani 1 1 d . U . . .
Re1 Re 0.47147(3) 0.80541(3) 0.39931(9) 0.02254(19) Uani 1 1 d . U . . .
N1 N 0.4238(14) 0.7254(10) 0.554(6) 0.031(2) Uani 0.414(15) 1 d D U P A 1
O1 O 0.4405(11) 0.6774(10) 0.507(4) 0.031(2) Uani 0.414(15) 1 d D U P A 1
O2 O 0.3819(12) 0.7348(11) 0.658(5) 0.031(2) Uani 0.414(15) 1 d D U P A 1
N1A N 0.3943(9) 0.7177(8) 0.633(4) 0.031(2) Uani 0.586(15) 1 d D U P A 2
O1A O 0.4418(8) 0.7280(8) 0.535(4) 0.031(2) Uani 0.586(15) 1 d D U P A 2
O2A O 0.3643(7) 0.7656(8) 0.651(3) 0.031(2) Uani 0.586(15) 1 d D U P A 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
C1 O3 1.174(18) . ?
C1 Re1 1.919(16) . ?
C2 O4 1.145(19) . ?
C2 Re1 1.925(17) . ?
C3 O5 1.139(18) . ?
C3 Re1 1.922(16) . ?
C4 C5 1.37(2) . ?
C4 N2 1.37(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(2) . ?
C5 H5 0.9300 . ?
C6 O6 1.359(18) . ?
C6 C7 1.41(2) . ?
C7 C8 1.38(2) . ?
C7 H7 0.9300 . ?
C8 N2 1.37(2) . ?
C8 C9 1.48(2) . ?
C9 N3 1.351(19) . ?
C9 C10 1.35(2) . ?
C10 C11 1.39(2) . ?
C10 H10 0.9300 . ?
C11 O7 1.355(19) . ?
C11 C12 1.41(2) . ?
C12 C13 1.38(2) . ?
C12 H12 0.9300 . ?
C13 N3 1.338(19) . ?
C13 H13 0.9300 . ?
C14 O6 1.444(17) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.420(19) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 Re1 2.166(12) . ?
N3 Re1 2.188(13) . ?
Re1 O1A 2.08(2) . ?
Re1 N1 2.35(2) . ?
N1 O2 1.187(13) . ?
N1 O1 1.196(13) . ?
N1A O1A 1.279(13) . ?
N1A O2A 1.289(13) . ?

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
O3 C1 Re1 177.7(13) . . ?
O4 C2 Re1 175.8(15) . . ?
O5 C3 Re1 178.7(16) . . ?
C5 C4 N2 122.7(15) . . ?
C5 C4 H4 118.6 . . ?
N2 C4 H4 118.6 . . ?
C4 C5 C6 119.9(14) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
O6 C6 C5 126.3(13) . . ?
O6 C6 C7 115.3(14) . . ?
C5 C6 C7 118.4(14) . . ?
C8 C7 C6 119.7(14) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N2 C8 C7 121.4(13) . . ?
N2 C8 C9 116.0(13) . . ?
C7 C8 C9 122.4(14) . . ?
N3 C9 C10 122.4(15) . . ?
N3 C9 C8 114.0(13) . . ?
C10 C9 C8 123.4(14) . . ?
C9 C10 C11 119.9(15) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
O7 C11 C10 117.9(15) . . ?
O7 C11 C12 123.5(14) . . ?
C10 C11 C12 118.6(16) . . ?
C13 C12 C11 117.3(15) . . ?
C13 C12 H12 121.3 . . ?
C11 C12 H12 121.3 . . ?
N3 C13 C12 123.7(15) . . ?
N3 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C8 N2 C4 117.6(13) . . ?
C8 N2 Re1 117.0(10) . . ?
C4 N2 Re1 125.4(11) . . ?
C13 N3 C9 117.9(14) . . ?
C13 N3 Re1 123.8(11) . . ?
C9 N3 Re1 117.7(10) . . ?
C6 O6 C14 116.2(13) . . ?
C11 O7 C15 118.0(13) . . ?
C1 Re1 C3 87.9(6) . . ?
C1 Re1 C2 88.0(7) . . ?
C3 Re1 C2 90.0(7) . . ?
C1 Re1 O1A 97.4(8) . . ?
C3 Re1 O1A 170.5(6) . . ?
C2 Re1 O1A 98.0(7) . . ?
C1 Re1 N2 175.2(6) . . ?
C3 Re1 N2 95.2(6) . . ?
C2 Re1 N2 95.7(6) . . ?
O1A Re1 N2 79.0(7) . . ?
C1 Re1 N3 101.5(6) . . ?
C3 Re1 N3 95.0(6) . . ?
C2 Re1 N3 169.4(6) . . ?
O1A Re1 N3 76.2(6) . . ?
N2 Re1 N3 74.6(5) . . ?
C1 Re1 N1 90.0(11) . . ?
C3 Re1 N1 176.4(11) . . ?
C2 Re1 N1 92.9(8) . . ?
N2 Re1 N1 86.7(10) . . ?
N3 Re1 N1 82.5(7) . . ?
O2 N1 O1 125(2) . . ?
O2 N1 Re1 118.4(18) . . ?
O1 N1 Re1 116.6(18) . . ?
O1A N1A O2A 109.8(13) . . ?
N1A O1A Re1 129.9(13) . . ?

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
N2 C4 C5 C6 -2(2) . . . . ?
C4 C5 C6 O6 -178.0(14) . . . . ?
C4 C5 C6 C7 4(2) . . . . ?
O6 C6 C7 C8 -179.7(13) . . . . ?
C5 C6 C7 C8 -2(2) . . . . ?
C6 C7 C8 N2 -3(2) . . . . ?
C6 C7 C8 C9 -177.9(14) . . . . ?
N2 C8 C9 N3 6(2) . . . . ?
C7 C8 C9 N3 -178.8(14) . . . . ?
N2 C8 C9 C10 -179.2(15) . . . . ?
C7 C8 C9 C10 -4(2) . . . . ?
N3 C9 C10 C11 -5(2) . . . . ?
C8 C9 C10 C11 -179.1(15) . . . . ?
C9 C10 C11 O7 -178.3(15) . . . . ?
C9 C10 C11 C12 4(2) . . . . ?
O7 C11 C12 C13 -179.5(15) . . . . ?
C10 C11 C12 C13 -2(2) . . . . ?
C11 C12 C13 N3 1(2) . . . . ?
C7 C8 N2 C4 5(2) . . . . ?
C9 C8 N2 C4 -179.7(13) . . . . ?
C7 C8 N2 Re1 -174.6(11) . . . . ?
C9 C8 N2 Re1 0.5(17) . . . . ?
C5 C4 N2 C8 -3(2) . . . . ?
C5 C4 N2 Re1 177.2(11) . . . . ?
C12 C13 N3 C9 -1(2) . . . . ?
C12 C13 N3 Re1 -172.8(12) . . . . ?
C10 C9 N3 C13 3(2) . . . . ?
C8 C9 N3 C13 177.9(13) . . . . ?
C10 C9 N3 Re1 175.3(12) . . . . ?
C8 C9 N3 Re1 -9.9(17) . . . . ?
C5 C6 O6 C14 -2(2) . . . . ?
C7 C6 O6 C14 176.4(14) . . . . ?
C10 C11 O7 C15 -179.6(16) . . . . ?
C12 C11 O7 C15 -2(2) . . . . ?
O2A N1A O1A Re1 -4(4) . . . . ?

_refine_diff_density_max         1.351
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.171


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_210K
_database_code_depnum_ccdc_archive 'CCDC 1842780'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT972_PSS_210K            
;
PROBLEM: Check Calcd Resid. Dens. 0.95A From Re1 -3.63 eA-3
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
_vrf_PLAT973_PSS_210K            
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 3.38 eA-3
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
_vrf_PLAT342_PSS_210K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.83 A)
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.7012(19)
_cell_length_b                   22.7012(19)
_cell_length_c                   6.5603(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3380.8(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    907
_cell_measurement_theta_min      3.5690
_cell_measurement_theta_max      22.1090

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.025
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 5 1 0.0110
-2 -5 -1 0.0223
5 5 -3 0.1429
-5 -5 3 0.1566
5 -3 1 0.0125
-5 3 -1 0.0125
_exptl_absorpt_coefficient_mu    7.233
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            5229
_diffrn_reflns_av_unetI/netI     0.1852
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.590
_diffrn_reflns_theta_max         25.313
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             2958
_reflns_number_gt                1766
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_max     0.902
_reflns_Friedel_fraction_full    0.902

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0694P)²+54.3816P] 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 374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2958
_refine_ls_number_parameters     241
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0957
_refine_ls_wR_factor_ref         0.2319
_refine_ls_wR_factor_gt          0.1880
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1791(19) 0.4014(19) 0.257(6) 0.050(4) Uani 1 1 d . U . . .
C2 C 0.1425(18) 0.4465(18) 0.594(7) 0.056(4) Uani 1 1 d . U . . .
C3 C 0.134(2) 0.506(2) 0.262(7) 0.054(5) Uani 1 1 d . U . . .
C4 C 0.198(2) 0.5707(19) 0.725(6) 0.052(8) Uani 1 1 d . U . . .
H4 H 0.1660 0.5504 0.7779 0.062 Uiso 1 1 calc R U . . .
C5 C 0.220(2) 0.6185(19) 0.825(7) 0.058(9) Uani 1 1 d . U . . .
H5 H 0.2012 0.6317 0.9427 0.069 Uiso 1 1 calc R U . . .
C6 C 0.2701(19) 0.6481(19) 0.756(6) 0.049(7) Uani 1 1 d . U . . .
C7 C 0.2928(19) 0.6288(18) 0.568(7) 0.056(9) Uani 1 1 d . U . . .
H7 H 0.3231 0.6498 0.5060 0.067 Uiso 1 1 calc R U . . .
C8 C 0.2713(18) 0.5803(18) 0.478(6) 0.043(7) Uani 1 1 d . U . . .
C9 C 0.293(2) 0.556(2) 0.281(6) 0.054(9) Uani 1 1 d . U . . .
C10 C 0.3406(17) 0.5785(17) 0.199(6) 0.041(7) Uani 1 1 d . U . . .
H10 H 0.3608 0.6089 0.2633 0.049 Uiso 1 1 calc R U . . .
C11 C 0.3609(18) 0.5557(19) 0.013(6) 0.043(7) Uani 1 1 d . U . . .
C12 C 0.3315(18) 0.5071(18) -0.074(7) 0.057(9) Uani 1 1 d . U . . .
H12 H 0.3434 0.4891 -0.1943 0.069 Uiso 1 1 calc R U . . .
C13 C 0.2825(18) 0.4885(19) 0.040(6) 0.051(8) Uani 1 1 d . U . . .
H13 H 0.2619 0.4569 -0.0152 0.061 Uiso 1 1 calc R U . . .
C14 C 0.269(2) 0.7187(18) 1.013(6) 0.055(9) Uani 1 1 d . U . . .
H14A H 0.2292 0.7296 0.9835 0.082 Uiso 1 1 calc R U . . .
H14B H 0.2908 0.7529 1.0554 0.082 Uiso 1 1 calc R U . . .
H14C H 0.2696 0.6899 1.1198 0.082 Uiso 1 1 calc R U . . .
C15 C 0.428(2) 0.554(2) -0.265(6) 0.078(15) Uani 1 1 d . U . . .
H15A H 0.3989 0.5608 -0.3682 0.117 Uiso 1 1 calc R U . . .
H15B H 0.4341 0.5124 -0.2492 0.117 Uiso 1 1 calc R U . . .
H15C H 0.4645 0.5723 -0.3050 0.117 Uiso 1 1 calc R U . . .
N2 N 0.2235(15) 0.5528(15) 0.548(5) 0.049(3) Uani 1 1 d . U . . .
N3 N 0.2612(15) 0.5096(15) 0.215(5) 0.050(3) Uani 1 1 d . U . . .
O0AA O 0.1655(13) 0.3569(13) 0.170(5) 0.074(10) Uani 1 1 d . U . . .
O3 O 0.1107(15) 0.4337(14) 0.740(5) 0.077(10) Uani 1 1 d . U . . .
O4 O 0.0937(16) 0.5307(16) 0.170(6) 0.093(12) Uani 1 1 d . U . . .
O5 O 0.2953(13) 0.6949(13) 0.837(4) 0.062(7) Uani 1 1 d . U . . .
O6 O 0.4090(14) 0.5781(14) -0.080(5) 0.071(8) Uani 1 1 d . U . . .
Re1 Re 0.19469(8) 0.47183(8) 0.3995(3) 0.0523(5) Uani 1 1 d . U . . .
N1 N 0.276(2) 0.4276(10) 0.553(2) 0.055(4) Uani 0.40(4) 1 d D U P A 1
O1 O 0.325(3) 0.445(2) 0.524(7) 0.057(4) Uani 0.40(4) 1 d D U P A 1
O2 O 0.266(3) 0.3824(13) 0.642(4) 0.057(4) Uani 0.40(4) 1 d D U P A 1
N1A N 0.2853(15) 0.3940(14) 0.621(5) 0.055(4) Uani 0.60(4) 1 d D U P A 2
O1A O 0.271(2) 0.4419(12) 0.525(3) 0.057(4) Uani 0.60(4) 1 d D U P A 2
O2A O 0.2369(19) 0.3669(15) 0.670(5) 0.057(4) Uani 0.60(4) 1 d D U P A 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
C1 O0AA 1.20(5) . ?
C1 Re1 1.89(4) . ?
C2 O3 1.23(5) . ?
C2 Re1 1.83(5) . ?
C3 O4 1.22(5) . ?
C3 Re1 1.83(4) . ?
C4 N2 1.36(5) . ?
C4 C5 1.36(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.40(6) . ?
C5 H5 0.9300 . ?
C6 O5 1.32(5) . ?
C6 C7 1.41(6) . ?
C7 C8 1.34(5) . ?
C7 H7 0.9300 . ?
C8 N2 1.33(5) . ?
C8 C9 1.48(5) . ?
C9 C10 1.31(5) . ?
C9 N3 1.35(5) . ?
C10 C11 1.40(5) . ?
C10 H10 0.9300 . ?
C11 O6 1.35(5) . ?
C11 C12 1.41(5) . ?
C12 C13 1.40(6) . ?
C12 H12 0.9300 . ?
C13 N3 1.34(5) . ?
C13 H13 0.9300 . ?
C14 O5 1.41(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O6 1.40(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 Re1 2.18(3) . ?
N3 Re1 2.12(3) . ?
Re1 O1A 2.04(4) . ?
Re1 N1 2.33(4) . ?
N1 O2 1.201(14) . ?
N1 O1 1.201(14) . ?
N1A O2A 1.298(14) . ?
N1A O1A 1.300(14) . ?

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
O0AA C1 Re1 176(4) . . ?
O3 C2 Re1 173(4) . . ?
O4 C3 Re1 179(4) . . ?
N2 C4 C5 120(4) . . ?
N2 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 122(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
O5 C6 C5 128(4) . . ?
O5 C6 C7 116(4) . . ?
C5 C6 C7 116(4) . . ?
C8 C7 C6 121(4) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N2 C8 C7 122(4) . . ?
N2 C8 C9 113(4) . . ?
C7 C8 C9 124(4) . . ?
C10 C9 N3 127(4) . . ?
C10 C9 C8 119(4) . . ?
N3 C9 C8 113(4) . . ?
C9 C10 C11 119(4) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
O6 C11 C10 121(4) . . ?
O6 C11 C12 120(4) . . ?
C10 C11 C12 119(4) . . ?
C13 C12 C11 113(4) . . ?
C13 C12 H12 123.3 . . ?
C11 C12 H12 123.3 . . ?
N3 C13 C12 129(4) . . ?
N3 C13 H13 115.3 . . ?
C12 C13 H13 115.3 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C8 N2 C4 120(4) . . ?
C8 N2 Re1 119(3) . . ?
C4 N2 Re1 121(3) . . ?
C13 N3 C9 111(4) . . ?
C13 N3 Re1 127(3) . . ?
C9 N3 Re1 121(3) . . ?
C6 O5 C14 117(4) . . ?
C11 O6 C15 120(3) . . ?
C3 Re1 C2 89(2) . . ?
C3 Re1 C1 88.7(18) . . ?
C2 Re1 C1 87.5(19) . . ?
C3 Re1 O1A 170.7(17) . . ?
C2 Re1 O1A 99.5(15) . . ?
C1 Re1 O1A 94.4(14) . . ?
C3 Re1 N3 94.7(16) . . ?
C2 Re1 N3 170.4(16) . . ?
C1 Re1 N3 101.2(16) . . ?
O1A Re1 N3 76.0(12) . . ?
C3 Re1 N2 95.0(16) . . ?
C2 Re1 N2 98.5(16) . . ?
C1 Re1 N2 173.0(16) . . ?
O1A Re1 N2 81.1(12) . . ?
N3 Re1 N2 72.6(13) . . ?
C3 Re1 N1 176.0(15) . . ?
C2 Re1 N1 94.3(16) . . ?
C1 Re1 N1 89.9(14) . . ?
N3 Re1 N1 81.9(13) . . ?
N2 Re1 N1 86.1(11) . . ?
O2 N1 O1 122(2) . . ?
O2 N1 Re1 116(3) . . ?
O1 N1 Re1 122(3) . . ?
O2A N1A O1A 107.8(15) . . ?
N1A O1A Re1 133(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 -3(7) . . . . ?
C4 C5 C6 O5 179(4) . . . . ?
C4 C5 C6 C7 6(6) . . . . ?
O5 C6 C7 C8 178(4) . . . . ?
C5 C6 C7 C8 -8(6) . . . . ?
C6 C7 C8 N2 8(7) . . . . ?
C6 C7 C8 C9 -179(4) . . . . ?
N2 C8 C9 C10 -178(4) . . . . ?
C7 C8 C9 C10 9(7) . . . . ?
N2 C8 C9 N3 -2(5) . . . . ?
C7 C8 C9 N3 -176(4) . . . . ?
N3 C9 C10 C11 5(7) . . . . ?
C8 C9 C10 C11 180(3) . . . . ?
C9 C10 C11 O6 178(4) . . . . ?
C9 C10 C11 C12 -4(6) . . . . ?
O6 C11 C12 C13 180(4) . . . . ?
C10 C11 C12 C13 2(6) . . . . ?
C11 C12 C13 N3 -1(7) . . . . ?
C7 C8 N2 C4 -6(6) . . . . ?
C9 C8 N2 C4 -179(3) . . . . ?
C7 C8 N2 Re1 -177(3) . . . . ?
C9 C8 N2 Re1 10(4) . . . . ?
C5 C4 N2 C8 3(6) . . . . ?
C5 C4 N2 Re1 174(3) . . . . ?
C12 C13 N3 C9 2(6) . . . . ?
C12 C13 N3 Re1 -170(3) . . . . ?
C10 C9 N3 C13 -4(7) . . . . ?
C8 C9 N3 C13 -179(3) . . . . ?
C10 C9 N3 Re1 169(4) . . . . ?
C8 C9 N3 Re1 -6(5) . . . . ?
C5 C6 O5 C14 0(6) . . . . ?
C7 C6 O5 C14 173(4) . . . . ?
C10 C11 O6 C15 180(4) . . . . ?
C12 C11 O6 C15 2(6) . . . . ?
O2A N1A O1A Re1 -12(5) . . . . ?

_refine_diff_density_max         2.367
_refine_diff_density_min         -4.223
_refine_diff_density_rms         0.267


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_MS_170K
_database_code_depnum_ccdc_archive 'CCDC 1842793'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT973_MS_170K             
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 2.01 eA-3
RESPONSE: Reduced data quality due to irradiation damage following a 3 h
continuous LED illumination period. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.6722(6)
_cell_length_b                   22.6722(6)
_cell_length_c                   6.5648(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3374.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    2916
_cell_measurement_theta_min      3.5820
_cell_measurement_theta_max      25.4400

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0093
-1 -1 0 0.0091
0 0 -1 0.1246
0 0 1 0.1246
1 1 0 0.0100
1 -1 0 0.0123
_exptl_absorpt_coefficient_mu    7.246
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            8014
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.841
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3440
_reflns_number_gt                2886
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.997

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0240P)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 1063 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3440
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0709
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0533(5) 0.1399(6) 0.355(2) 0.037(2) Uani 1 1 d . U . . .
C2 C 0.1004(6) 0.1763(6) 0.004(2) 0.033(3) Uani 1 1 d . U . . .
C3 C -0.0096(6) 0.1311(6) 0.008(2) 0.035(3) Uani 1 1 d . U . . .
C4 C 0.0141(6) 0.2829(6) -0.2126(19) 0.033(3) Uani 1 1 d . U . . .
H4 H 0.0468 0.2621 -0.2669 0.040 Uiso 1 1 calc R U . . .
C5 C -0.0060(5) 0.3307(5) -0.320(2) 0.033(3) Uani 1 1 d . U . . .
H5 H 0.0123 0.3428 -0.4438 0.040 Uiso 1 1 calc R U . . .
C6 C -0.0544(6) 0.3607(6) -0.241(2) 0.035(3) Uani 1 1 d . U . . .
C7 C -0.0792(6) 0.3416(6) -0.062(2) 0.032(3) Uani 1 1 d . U . . .
H7 H -0.1123 0.3616 -0.0058 0.038 Uiso 1 1 calc R U . . .
C8 C -0.0560(6) 0.2935(5) 0.037(2) 0.030(2) Uani 1 1 d . U . . .
C9 C -0.0798(5) 0.2700(5) 0.228(2) 0.028(2) Uani 1 1 d . U . . .
C10 C -0.1281(5) 0.2935(5) 0.3247(19) 0.028(2) Uani 1 1 d . U . . .
H10 H -0.1480 0.3264 0.2670 0.034 Uiso 1 1 calc R U . . .
C11 C -0.1482(5) 0.2694(6) 0.5066(19) 0.029(2) Uani 1 1 d . U . . .
C12 C -0.1203(5) 0.2200(6) 0.581(2) 0.033(3) Uani 1 1 d . U . . .
H12 H -0.1339 0.2010 0.7013 0.039 Uiso 1 1 calc R U . . .
C13 C -0.0715(5) 0.1985(6) 0.476(2) 0.033(3) Uani 1 1 d . U . . .
H13 H -0.0522 0.1646 0.5282 0.040 Uiso 1 1 calc R U . . .
C14 C -0.0540(7) 0.4299(7) -0.516(2) 0.052(4) Uani 1 1 d . U . . .
H14A H -0.0127 0.4409 -0.4948 0.079 Uiso 1 1 calc R U . . .
H14B H -0.0763 0.4644 -0.5621 0.079 Uiso 1 1 calc R U . . .
H14C H -0.0563 0.3988 -0.6195 0.079 Uiso 1 1 calc R U . . .
C15 C -0.2192(6) 0.2693(6) 0.774(2) 0.039(3) Uani 1 1 d . U . . .
H15A H -0.1880 0.2657 0.8763 0.059 Uiso 1 1 calc R U . . .
H15B H -0.2350 0.2301 0.7424 0.059 Uiso 1 1 calc R U . . .
H15C H -0.2509 0.2944 0.8267 0.059 Uiso 1 1 calc R U . . .
N2 N -0.0085(4) 0.2634(4) -0.0380(16) 0.0304(18) Uani 1 1 d . U . . .
N3 N -0.0505(4) 0.2228(4) 0.3079(17) 0.0301(19) Uani 1 1 d . U . . .
O3 O 0.0656(4) 0.1083(5) 0.4845(16) 0.055(3) Uani 1 1 d . U . . .
O4 O 0.1428(4) 0.1652(4) -0.0802(15) 0.048(3) Uani 1 1 d . U . . .
O5 O -0.0321(4) 0.0943(5) -0.0787(16) 0.058(3) Uani 1 1 d . U . . .
O6 O -0.0785(4) 0.4086(4) -0.3283(16) 0.049(2) Uani 1 1 d . U . . .
O7 O -0.1955(4) 0.2951(4) 0.5924(12) 0.039(2) Uani 1 1 d . U . . .
Re1 Re 0.02854(2) 0.19459(2) 0.14954(8) 0.03088(16) Uani 1 1 d . U . . .
N1 N 0.0756(15) 0.2741(9) 0.304(6) 0.0404(19) Uani 0.401(12) 1 d D U P A 1
O1 O 0.0604(9) 0.3232(9) 0.260(3) 0.0404(19) Uani 0.401(12) 1 d D U P A 1
O2 O 0.1166(11) 0.2648(10) 0.412(4) 0.0404(19) Uani 0.401(12) 1 d D U P A 1
N1A N 0.1063(8) 0.2829(7) 0.381(4) 0.0404(19) Uani 0.599(12) 1 d D U P A 2
O1A O 0.0585(7) 0.2723(7) 0.284(3) 0.0404(19) Uani 0.599(12) 1 d D U P A 2
O2A O 0.1367(6) 0.2350(6) 0.400(2) 0.0404(19) Uani 0.599(12) 1 d D U P A 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
C1 O3 1.148(15) . ?
C1 Re1 1.915(15) . ?
C2 O4 1.138(14) . ?
C2 Re1 1.933(14) . ?
C3 O5 1.134(15) . ?
C3 Re1 1.918(14) . ?
C4 N2 1.331(15) . ?
C4 C5 1.372(17) . ?
C5 C6 1.391(17) . ?
C6 O6 1.343(16) . ?
C6 C7 1.379(18) . ?
C7 C8 1.370(18) . ?
C8 N2 1.366(15) . ?
C8 C9 1.467(17) . ?
C9 N3 1.367(16) . ?
C9 C10 1.374(16) . ?
C10 C11 1.390(17) . ?
C11 O7 1.344(14) . ?
C11 C12 1.377(17) . ?
C12 C13 1.391(17) . ?
C13 N3 1.322(17) . ?
C14 O6 1.435(16) . ?
C15 O7 1.431(15) . ?
N2 Re1 2.158(11) . ?
N3 Re1 2.168(10) . ?
Re1 O1A 2.085(16) . ?
Re1 N1 2.33(3) . ?
N1 O2 1.19(3) . ?
N1 O1 1.202(10) . ?
N1A O1A 1.281(13) . ?
N1A O2A 1.293(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
O3 C1 Re1 176.0(12) . . ?
O4 C2 Re1 179.2(13) . . ?
O5 C3 Re1 178.6(13) . . ?
N2 C4 C5 125.4(13) . . ?
C4 C5 C6 117.1(13) . . ?
O6 C6 C7 116.9(13) . . ?
O6 C6 C5 123.9(13) . . ?
C7 C6 C5 119.2(13) . . ?
C8 C7 C6 119.7(13) . . ?
N2 C8 C7 122.2(12) . . ?
N2 C8 C9 114.5(11) . . ?
C7 C8 C9 123.3(12) . . ?
N3 C9 C10 120.9(12) . . ?
N3 C9 C8 115.8(11) . . ?
C10 C9 C8 123.3(12) . . ?
C9 C10 C11 120.5(12) . . ?
O7 C11 C12 124.8(12) . . ?
O7 C11 C10 116.8(11) . . ?
C12 C11 C10 118.3(12) . . ?
C11 C12 C13 118.3(12) . . ?
N3 C13 C12 123.8(13) . . ?
C4 N2 C8 116.4(11) . . ?
C4 N2 Re1 125.6(9) . . ?
C8 N2 Re1 117.7(8) . . ?
C13 N3 C9 118.1(12) . . ?
C13 N3 Re1 125.2(9) . . ?
C9 N3 Re1 116.7(8) . . ?
C6 O6 C14 118.6(11) . . ?
C11 O7 C15 118.1(10) . . ?
C1 Re1 C3 89.2(6) . . ?
C1 Re1 C2 87.8(6) . . ?
C3 Re1 C2 88.9(5) . . ?
C1 Re1 O1A 98.9(6) . . ?
C3 Re1 O1A 170.3(6) . . ?
C2 Re1 O1A 96.6(6) . . ?
C1 Re1 N2 169.7(5) . . ?
C3 Re1 N2 95.2(5) . . ?
C2 Re1 N2 101.6(5) . . ?
O1A Re1 N2 75.9(5) . . ?
C1 Re1 N3 95.5(5) . . ?
C3 Re1 N3 94.6(5) . . ?
C2 Re1 N3 175.2(5) . . ?
O1A Re1 N3 79.5(6) . . ?
N2 Re1 N3 74.9(4) . . ?
C1 Re1 N1 93.5(8) . . ?
C3 Re1 N1 176.9(10) . . ?
C2 Re1 N1 89.7(10) . . ?
N2 Re1 N1 82.3(7) . . ?
N3 Re1 N1 86.7(10) . . ?
O2 N1 O1 122(3) . . ?
O2 N1 Re1 118.8(17) . . ?
O1 N1 Re1 119(2) . . ?
O1A N1A O2A 109.9(13) . . ?
N1A O1A Re1 130.2(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
N2 C4 C5 C6 -0.7(19) . . . . ?
C4 C5 C6 O6 179.1(12) . . . . ?
C4 C5 C6 C7 0.2(19) . . . . ?
O6 C6 C7 C8 -178.8(12) . . . . ?
C5 C6 C7 C8 0.1(19) . . . . ?
C6 C7 C8 N2 0(2) . . . . ?
C6 C7 C8 C9 -179.6(12) . . . . ?
N2 C8 C9 N3 2.0(15) . . . . ?
C7 C8 C9 N3 -178.4(12) . . . . ?
N2 C8 C9 C10 -178.8(12) . . . . ?
C7 C8 C9 C10 0.9(19) . . . . ?
N3 C9 C10 C11 -0.2(18) . . . . ?
C8 C9 C10 C11 -179.4(11) . . . . ?
C9 C10 C11 O7 179.7(11) . . . . ?
C9 C10 C11 C12 -3.0(18) . . . . ?
O7 C11 C12 C13 -179.7(11) . . . . ?
C10 C11 C12 C13 3.2(18) . . . . ?
C11 C12 C13 N3 -0.3(19) . . . . ?
C5 C4 N2 C8 0.7(18) . . . . ?
C5 C4 N2 Re1 -172.8(9) . . . . ?
C7 C8 N2 C4 -0.4(18) . . . . ?
C9 C8 N2 C4 179.3(11) . . . . ?
C7 C8 N2 Re1 173.7(10) . . . . ?
C9 C8 N2 Re1 -6.7(13) . . . . ?
C12 C13 N3 C9 -3.0(18) . . . . ?
C12 C13 N3 Re1 175.8(9) . . . . ?
C10 C9 N3 C13 3.2(18) . . . . ?
C8 C9 N3 C13 -177.5(11) . . . . ?
C10 C9 N3 Re1 -175.7(9) . . . . ?
C8 C9 N3 Re1 3.6(14) . . . . ?
C7 C6 O6 C14 -179.8(13) . . . . ?
C5 C6 O6 C14 1(2) . . . . ?
C12 C11 O7 C15 -0.5(17) . . . . ?
C10 C11 O7 C15 176.6(11) . . . . ?
O2A N1A O1A Re1 -4(3) . . . . ?

_refine_diff_density_max         1.596
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.150


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_200K
_database_code_depnum_ccdc_archive 'CCDC 1842781'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT342_PSS_200K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03333 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.83 A)
;
# end Validation Reply Form


_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.738(2)
_cell_length_b                   22.738(2)
_cell_length_c                   6.5434(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3383.0(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2221
_cell_measurement_theta_min      3.5570
_cell_measurement_theta_max      27.7440

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
1 1 1 0.1206
-1 -1 -1 0.1391
-1 1 0 0.0116
-1 -1 0 0.0096
1 1 0 0.0096
_exptl_absorpt_coefficient_mu    7.228
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            5957
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.833
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.936
_reflns_number_total             2899
_reflns_number_gt                2461
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_max     0.855
_reflns_Friedel_fraction_full    0.861

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0902P)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 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.04(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2899
_refine_ls_number_parameters     235
_refine_ls_number_restraints     259
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1663
_refine_ls_wR_factor_gt          0.1559
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5977(11) 0.3224(11) -0.003(4) 0.031(3) Uani 1 1 d . U . . .
C2 C 0.5518(11) 0.3597(11) 0.358(4) 0.035(3) Uani 1 1 d . U . . .
C3 C 0.4905(11) 0.3702(11) 0.007(4) 0.030(4) Uani 1 1 d . U . . .
C4 C 0.4280(11) 0.3025(12) 0.479(4) 0.031(4) Uani 1 1 d . U . . .
H4 H 0.4474 0.3351 0.5325 0.037 Uiso 1 1 calc R U . . .
C5 C 0.3787(10) 0.2816(11) 0.579(4) 0.031(4) Uani 1 1 d . U . . .
H5 H 0.3642 0.3010 0.6938 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3513(10) 0.2312(11) 0.507(3) 0.025(4) Uani 1 1 d . U . . .
C7 C 0.3713(9) 0.2074(10) 0.324(3) 0.025(4) Uani 1 1 d . U . . .
H7 H 0.3516 0.1757 0.2659 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4186(10) 0.2297(10) 0.231(3) 0.022(3) Uani 1 1 d . U . . .
C9 C 0.4435(10) 0.2073(10) 0.041(4) 0.026(4) Uani 1 1 d . U . . .
C10 C 0.4195(13) 0.1576(13) -0.064(4) 0.040(6) Uani 1 1 d . U . . .
H10 H 0.3870 0.1378 -0.0115 0.048 Uiso 1 1 calc R U . . .
C11 C 0.4454(12) 0.1395(11) -0.243(4) 0.029(4) Uani 1 1 d . U . . .
C12 C 0.4924(11) 0.1697(10) -0.318(4) 0.031(4) Uani 1 1 d . U . . .
H12 H 0.5100 0.1581 -0.4399 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5138(12) 0.2175(11) -0.212(3) 0.031(4) Uani 1 1 d . U . . .
H13 H 0.5465 0.2372 -0.2631 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2813(13) 0.2316(15) 0.775(4) 0.052(8) Uani 1 1 d . U . . .
H14A H 0.3120 0.2358 0.8748 0.078 Uiso 1 1 calc R U . . .
H14B H 0.2506 0.2073 0.8302 0.078 Uiso 1 1 calc R U . . .
H14C H 0.2656 0.2697 0.7425 0.078 Uiso 1 1 calc R U . . .
C15 C 0.4451(16) 0.0699(16) -0.517(5) 0.067(10) Uani 1 1 d . U . . .
H15A H 0.4833 0.0533 -0.4926 0.100 Uiso 1 1 calc R U . . .
H15B H 0.4484 0.1017 -0.6124 0.100 Uiso 1 1 calc R U . . .
H15C H 0.4195 0.0402 -0.5716 0.100 Uiso 1 1 calc R U . . .
N2 N 0.4492(9) 0.2779(9) 0.306(3) 0.027(2) Uani 1 1 d . U . . .
N3 N 0.4894(9) 0.2362(9) -0.041(3) 0.030(2) Uani 1 1 d . U . . .
O3 O 0.6409(8) 0.3339(8) -0.081(3) 0.047(5) Uani 1 1 d . U . . .
O4 O 0.5651(10) 0.3909(10) 0.479(3) 0.056(6) Uani 1 1 d . U . . .
O5 O 0.4677(10) 0.4057(10) -0.080(3) 0.060(6) Uani 1 1 d . U . . .
O6 O 0.3047(8) 0.2049(9) 0.594(2) 0.042(4) Uani 1 1 d . U . . .
O7 O 0.4215(9) 0.0913(9) -0.329(3) 0.052(5) Uani 1 1 d . U . . .
Re1 Re 0.52751(4) 0.30529(4) 0.14819(14) 0.0289(3) Uani 1 1 d . U . . .
N1 N 0.575(2) 0.226(2) 0.298(9) 0.035(3) Uani 0.36(2) 1 d D U P A 1
O1 O 0.560(2) 0.1765(18) 0.269(7) 0.035(3) Uani 0.36(2) 1 d D U P A 1
O2 O 0.616(2) 0.235(2) 0.409(8) 0.035(3) Uani 0.36(2) 1 d D U P A 1
N1A N 0.6043(12) 0.2169(11) 0.376(6) 0.035(3) Uani 0.64(2) 1 d D U P A 2
O1A O 0.5548(11) 0.2278(13) 0.287(5) 0.035(3) Uani 0.64(2) 1 d D U P A 2
O2A O 0.6366(11) 0.2633(11) 0.397(4) 0.035(3) Uani 0.64(2) 1 d D U P A 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
C1 O3 1.14(3) . ?
C1 Re1 1.92(2) . ?
C2 O4 1.10(3) . ?
C2 Re1 1.93(3) . ?
C3 O5 1.12(3) . ?
C3 Re1 1.93(2) . ?
C4 N2 1.35(3) . ?
C4 C5 1.38(3) . ?
C5 C6 1.39(3) . ?
C6 O6 1.34(3) . ?
C6 C7 1.39(3) . ?
C7 C8 1.34(3) . ?
C8 N2 1.39(3) . ?
C8 C9 1.45(3) . ?
C9 N3 1.35(3) . ?
C9 C10 1.43(4) . ?
C10 C11 1.38(4) . ?
C11 O7 1.35(3) . ?
C11 C12 1.36(3) . ?
C12 C13 1.38(3) . ?
C13 N3 1.32(3) . ?
C14 O6 1.44(3) . ?
C15 O7 1.43(3) . ?
N2 Re1 2.151(19) . ?
N3 Re1 2.18(2) . ?
Re1 O1A 2.08(3) . ?
Re1 N1 2.32(5) . ?
N1 O2 1.197(14) . ?
N1 O1 1.198(14) . ?
N1A O1A 1.290(13) . ?
N1A O2A 1.294(13) . ?

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
O3 C1 Re1 175(2) . . ?
O4 C2 Re1 179(3) . . ?
O5 C3 Re1 176(2) . . ?
N2 C4 C5 123(2) . . ?
C4 C5 C6 119(2) . . ?
O6 C6 C5 125(2) . . ?
O6 C6 C7 117(2) . . ?
C5 C6 C7 118(2) . . ?
C8 C7 C6 121(2) . . ?
C7 C8 N2 123(2) . . ?
C7 C8 C9 125(2) . . ?
N2 C8 C9 113(2) . . ?
N3 C9 C10 119(2) . . ?
N3 C9 C8 118(2) . . ?
C10 C9 C8 123(2) . . ?
C11 C10 C9 119(2) . . ?
O7 C11 C12 125(2) . . ?
O7 C11 C10 115(2) . . ?
C12 C11 C10 119(3) . . ?
C11 C12 C13 120(2) . . ?
N3 C13 C12 122(2) . . ?
C4 N2 C8 116(2) . . ?
C4 N2 Re1 125.3(17) . . ?
C8 N2 Re1 118.2(15) . . ?
C13 N3 C9 121(2) . . ?
C13 N3 Re1 123.3(17) . . ?
C9 N3 Re1 115.5(16) . . ?
C6 O6 C14 117(2) . . ?
C11 O7 C15 119(2) . . ?
C1 Re1 C2 90.0(11) . . ?
C1 Re1 C3 87.8(10) . . ?
C2 Re1 C3 88.5(11) . . ?
C1 Re1 O1A 98.6(11) . . ?
C2 Re1 O1A 98.4(11) . . ?
C3 Re1 O1A 170.5(11) . . ?
C1 Re1 N2 174.6(10) . . ?
C2 Re1 N2 94.6(9) . . ?
C3 Re1 N2 95.1(9) . . ?
O1A Re1 N2 77.9(10) . . ?
C1 Re1 N3 100.5(9) . . ?
C2 Re1 N3 168.7(9) . . ?
C3 Re1 N3 96.0(9) . . ?
O1A Re1 N3 76.0(10) . . ?
N2 Re1 N3 74.7(8) . . ?
C1 Re1 N1 89.2(18) . . ?
C2 Re1 N1 93.5(14) . . ?
C3 Re1 N1 176.3(19) . . ?
N2 Re1 N1 87.7(16) . . ?
N3 Re1 N1 82.5(12) . . ?
O2 N1 O1 118(6) . . ?
O2 N1 Re1 120(4) . . ?
O1 N1 Re1 122(4) . . ?
O1A N1A O2A 113(3) . . ?
N1A O1A Re1 128(2) . . ?

_refine_diff_density_max         2.442
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.222


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_230K
_database_code_depnum_ccdc_archive 'CCDC 1842791'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.3673(5)
_cell_length_b                   22.3673(5)
_cell_length_c                   6.6855(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3344.73(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    3397
_cell_measurement_theta_min      3.6360
_cell_measurement_theta_max      27.6750

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.022
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0110
1 1 0 0.0110
-1 1 0 0.0214
1 -1 0 0.0116
-1 -2 1 0.1131
1 1 -1 0.1515
2 -1 2 0.1260
_exptl_absorpt_coefficient_mu    7.311
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6911
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.880
_diffrn_reflns_theta_max         25.341
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             2995
_reflns_number_gt                2711
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_max     0.955
_reflns_Friedel_fraction_full    0.959

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0305P)²+22.1261P] 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 1096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2995
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.033
_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
C1 C 0.1745(6) 0.6061(6) 0.735(2) 0.034(3) Uani 1 1 d . U . . .
C2 C 0.1387(6) 0.5588(6) 0.381(2) 0.038(3) Uani 1 1 d . U . . .
C3 C 0.1320(6) 0.4931(6) 0.727(2) 0.036(3) Uani 1 1 d . U . . .
C4 C 0.2017(6) 0.4344(6) 0.262(2) 0.034(3) Uani 1 1 d . U . . .
H4 H 0.1699 0.4549 0.2045 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2230(6) 0.3843(6) 0.166(2) 0.032(3) Uani 1 1 d . U . . .
H5 H 0.2057 0.3715 0.0473 0.039 Uiso 1 1 calc R U . . .
C6 C 0.2699(6) 0.3535(6) 0.248(2) 0.027(2) Uani 1 1 d . U . . .
C7 C 0.2940(6) 0.3744(5) 0.431(2) 0.028(2) Uani 1 1 d . U . . .
H7 H 0.3251 0.3538 0.4926 0.033 Uiso 1 1 calc R U . . .
C8 C 0.2711(6) 0.4251(6) 0.5158(19) 0.026(2) Uani 1 1 d . U . . .
C9 C 0.2938(6) 0.4495(6) 0.7081(19) 0.027(2) Uani 1 1 d . U . . .
C10 C 0.3405(6) 0.4253(6) 0.809(2) 0.033(3) Uani 1 1 d . U . . .
H10 H 0.3595 0.3913 0.7608 0.039 Uiso 1 1 calc R U . . .
C11 C 0.3600(6) 0.4520(7) 0.988(2) 0.033(3) Uani 1 1 d . U . . .
C12 C 0.3310(6) 0.5012(6) 1.055(2) 0.031(3) Uani 1 1 d . U . . .
H12 H 0.3433 0.5199 1.1722 0.037 Uiso 1 1 calc R U . . .
C13 C 0.2831(6) 0.5234(6) 0.9482(19) 0.031(3) Uani 1 1 d . U . . .
H13 H 0.2635 0.5572 0.9963 0.037 Uiso 1 1 calc R U . . .
C14 C 0.2690(7) 0.2792(7) -0.006(2) 0.039(4) Uani 1 1 d . U . . .
H14A H 0.2694 0.3084 -0.1113 0.058 Uiso 1 1 calc R U . . .
H14B H 0.2285 0.2679 0.0224 0.058 Uiso 1 1 calc R U . . .
H14C H 0.2912 0.2446 -0.0476 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4270(7) 0.4520(7) 1.260(2) 0.048(4) Uani 1 1 d . U . . .
H15A H 0.4419 0.4916 1.2361 0.072 Uiso 1 1 calc R U . . .
H15B H 0.4582 0.4278 1.3163 0.072 Uiso 1 1 calc R U . . .
H15C H 0.3941 0.4539 1.3519 0.072 Uiso 1 1 calc R U . . .
N1 N 0.2702(5) 0.5813(5) 0.4420(18) 0.034(2) Uani 1 1 d . U . . .
N2 N 0.2250(5) 0.4551(5) 0.4347(18) 0.0276(19) Uani 1 1 d . U . . .
N3 N 0.2633(5) 0.4981(5) 0.7761(16) 0.0275(19) Uani 1 1 d . U . . .
O1 O 0.3223(5) 0.5649(5) 0.4801(17) 0.051(3) Uani 1 1 d . U . . .
O2 O 0.2622(5) 0.6218(5) 0.3293(17) 0.057(3) Uani 1 1 d . U . . .
O3 O 0.1609(5) 0.6485(5) 0.8189(16) 0.052(3) Uani 1 1 d . U . . .
O4 O 0.1079(6) 0.5699(5) 0.255(2) 0.072(4) Uani 1 1 d . U . . .
O5 O 0.0953(6) 0.4702(5) 0.818(2) 0.073(4) Uani 1 1 d . U . . .
O6 O 0.2961(5) 0.3042(4) 0.1715(13) 0.037(2) Uani 1 1 d . U . . .
O7 O 0.4076(5) 0.4265(5) 1.0771(17) 0.048(3) Uani 1 1 d . U . . .
Re1 Re 0.19421(2) 0.53506(2) 0.58733(8) 0.02921(16) Uani 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 O3 1.143(16) . ?
C1 Re1 1.922(14) . ?
C2 O4 1.117(18) . ?
C2 Re1 1.928(15) . ?
C3 O5 1.140(17) . ?
C3 Re1 1.921(15) . ?
C4 N2 1.35(2) . ?
C4 C5 1.374(19) . ?
C4 H4 0.9300 . ?
C5 C6 1.369(19) . ?
C5 H5 0.9300 . ?
C6 O6 1.348(15) . ?
C6 C7 1.415(19) . ?
C7 C8 1.369(18) . ?
C7 H7 0.9300 . ?
C8 N2 1.344(17) . ?
C8 C9 1.486(18) . ?
C9 C10 1.358(18) . ?
C9 N3 1.362(16) . ?
C10 C11 1.402(19) . ?
C10 H10 0.9300 . ?
C11 O7 1.347(17) . ?
C11 C12 1.357(19) . ?
C12 C13 1.380(18) . ?
C12 H12 0.9300 . ?
C13 N3 1.357(17) . ?
C13 H13 0.9300 . ?
C14 O6 1.446(15) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.418(18) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N1 O2 1.193(15) . ?
N1 O1 1.249(15) . ?
N1 Re1 2.214(11) . ?
N2 Re1 2.172(11) . ?
N3 Re1 2.159(11) . ?

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
O3 C1 Re1 177.5(14) . . ?
O4 C2 Re1 175.9(14) . . ?
O5 C3 Re1 176.6(14) . . ?
N2 C4 C5 122.9(14) . . ?
N2 C4 H4 118.5 . . ?
C5 C4 H4 118.5 . . ?
C6 C5 C4 119.4(13) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
O6 C6 C5 126.3(12) . . ?
O6 C6 C7 115.6(12) . . ?
C5 C6 C7 118.0(12) . . ?
C8 C7 C6 119.3(12) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
N2 C8 C7 122.3(12) . . ?
N2 C8 C9 115.3(12) . . ?
C7 C8 C9 122.4(12) . . ?
C10 C9 N3 122.5(12) . . ?
C10 C9 C8 123.3(12) . . ?
N3 C9 C8 114.3(11) . . ?
C9 C10 C11 119.7(13) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
O7 C11 C12 125.1(13) . . ?
O7 C11 C10 116.3(13) . . ?
C12 C11 C10 118.6(14) . . ?
C11 C12 C13 119.5(13) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N3 C13 C12 122.8(12) . . ?
N3 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 119.5(13) . . ?
O2 N1 Re1 121.1(10) . . ?
O1 N1 Re1 119.4(9) . . ?
C8 N2 C4 118.1(12) . . ?
C8 N2 Re1 117.7(9) . . ?
C4 N2 Re1 124.2(10) . . ?
C13 N3 C9 117.0(11) . . ?
C13 N3 Re1 124.7(9) . . ?
C9 N3 Re1 118.0(8) . . ?
C6 O6 C14 116.6(11) . . ?
C11 O7 C15 117.1(11) . . ?
C3 Re1 C1 89.3(6) . . ?
C3 Re1 C2 90.9(7) . . ?
C1 Re1 C2 89.5(6) . . ?
C3 Re1 N3 92.7(5) . . ?
C1 Re1 N3 100.4(5) . . ?
C2 Re1 N3 169.5(5) . . ?
C3 Re1 N2 93.2(5) . . ?
C1 Re1 N2 174.4(6) . . ?
C2 Re1 N2 95.5(5) . . ?
N3 Re1 N2 74.5(4) . . ?
C3 Re1 N1 176.1(6) . . ?
C1 Re1 N1 90.9(5) . . ?
C2 Re1 N1 93.0(5) . . ?
N3 Re1 N1 83.5(4) . . ?
N2 Re1 N1 86.3(4) . . ?

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
N2 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 O6 -179.2(13) . . . . ?
C4 C5 C6 C7 1(2) . . . . ?
O6 C6 C7 C8 178.2(12) . . . . ?
C5 C6 C7 C8 -1.9(19) . . . . ?
C6 C7 C8 N2 2.0(19) . . . . ?
C6 C7 C8 C9 179.6(11) . . . . ?
N2 C8 C9 C10 -179.1(12) . . . . ?
C7 C8 C9 C10 3.2(19) . . . . ?
N2 C8 C9 N3 1.5(16) . . . . ?
C7 C8 C9 N3 -176.2(12) . . . . ?
N3 C9 C10 C11 -2(2) . . . . ?
C8 C9 C10 C11 178.5(12) . . . . ?
C9 C10 C11 O7 -178.4(13) . . . . ?
C9 C10 C11 C12 1(2) . . . . ?
O7 C11 C12 C13 179.3(13) . . . . ?
C10 C11 C12 C13 1(2) . . . . ?
C11 C12 C13 N3 0(2) . . . . ?
C7 C8 N2 C4 -1.1(19) . . . . ?
C9 C8 N2 C4 -178.8(12) . . . . ?
C7 C8 N2 Re1 -179.7(10) . . . . ?
C9 C8 N2 Re1 2.6(14) . . . . ?
C5 C4 N2 C8 0(2) . . . . ?
C5 C4 N2 Re1 178.5(10) . . . . ?
C12 C13 N3 C9 -1.3(18) . . . . ?
C12 C13 N3 Re1 -174.0(9) . . . . ?
C10 C9 N3 C13 2.4(18) . . . . ?
C8 C9 N3 C13 -178.1(11) . . . . ?
C10 C9 N3 Re1 175.6(10) . . . . ?
C8 C9 N3 Re1 -4.9(14) . . . . ?
C5 C6 O6 C14 -4.9(19) . . . . ?
C7 C6 O6 C14 175.0(12) . . . . ?
C12 C11 O7 C15 3(2) . . . . ?
C10 C11 O7 C15 -178.6(13) . . . . ?

_refine_diff_density_max         1.471
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.135


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_250K
_database_code_depnum_ccdc_archive 'CCDC 1842792'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.3700(6)
_cell_length_b                   22.3700(6)
_cell_length_c                   6.6942(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3349.9(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    2862
_cell_measurement_theta_min      3.1800
_cell_measurement_theta_max      26.6560

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.022
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0110
-1 1 0 0.0214
1 -1 0 0.0116
1 -2 -2 0.1260
-1 -1 1 0.1515
2 1 -1 0.1131
-1 -1 0 0.0110
_exptl_absorpt_coefficient_mu    7.300
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6895
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.879
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             2998
_reflns_number_gt                2681
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_max     0.954
_reflns_Friedel_fraction_full    0.958

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+23.1693P] 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 1075 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2998
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.037
_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
C1 C 0.6388(6) 0.4415(6) 0.134(2) 0.043(3) Uani 1 1 d . U . . .
C2 C 0.6743(6) 0.3938(6) 0.487(2) 0.036(3) Uani 1 1 d . U . . .
C3 C 0.6323(7) 0.5066(7) 0.474(3) 0.042(3) Uani 1 1 d . U . . .
C4 C 0.7827(6) 0.4767(6) 0.698(2) 0.037(3) Uani 1 1 d . U . . .
H4 H 0.7628 0.4433 0.7461 0.044 Uiso 1 1 calc R U . . .
C5 C 0.8309(6) 0.4989(6) 0.805(2) 0.033(3) Uani 1 1 d . U . . .
H5 H 0.8435 0.4802 0.9220 0.040 Uiso 1 1 calc R U . . .
C6 C 0.8593(6) 0.5481(6) 0.736(2) 0.033(3) Uani 1 1 d . U . . .
C7 C 0.8404(6) 0.5753(6) 0.558(2) 0.032(3) Uani 1 1 d . U . . .
H7 H 0.8593 0.6094 0.5100 0.039 Uiso 1 1 calc R U . . .
C8 C 0.7937(6) 0.5504(6) 0.4568(19) 0.030(2) Uani 1 1 d . U . . .
C9 C 0.7714(6) 0.5751(6) 0.2659(19) 0.028(2) Uani 1 1 d . U . . .
C10 C 0.7935(6) 0.6255(5) 0.180(2) 0.030(2) Uani 1 1 d . U . . .
H10 H 0.8247 0.6460 0.2415 0.036 Uiso 1 1 calc R U . . .
C11 C 0.7699(6) 0.6467(6) 0.000(2) 0.030(2) Uani 1 1 d . U . . .
C12 C 0.7230(6) 0.6156(6) -0.083(2) 0.036(3) Uani 1 1 d . U . . .
H12 H 0.7062 0.6284 -0.2030 0.043 Uiso 1 1 calc R U . . .
C13 C 0.7012(6) 0.5657(6) 0.010(2) 0.035(3) Uani 1 1 d . U . . .
H13 H 0.6690 0.5457 -0.0464 0.042 Uiso 1 1 calc R U . . .
C14 C 0.9269(7) 0.5482(7) 1.010(2) 0.052(4) Uani 1 1 d . U . . .
H14A H 0.9398 0.5078 0.9881 0.078 Uiso 1 1 calc R U . . .
H14B H 0.8946 0.5486 1.1041 0.078 Uiso 1 1 calc R U . . .
H14C H 0.9596 0.5714 1.0611 0.078 Uiso 1 1 calc R U . . .
C15 C 0.7693(7) 0.7201(7) -0.255(2) 0.041(4) Uani 1 1 d . U . . .
H15A H 0.7691 0.6905 -0.3588 0.061 Uiso 1 1 calc R U . . .
H15B H 0.7918 0.7542 -0.2979 0.061 Uiso 1 1 calc R U . . .
H15C H 0.7289 0.7320 -0.2263 0.061 Uiso 1 1 calc R U . . .
N1 N 0.7699(5) 0.4188(5) 0.1909(19) 0.037(2) Uani 1 1 d . U . . .
N2 N 0.7635(5) 0.5019(5) 0.5244(16) 0.0304(19) Uani 1 1 d . U . . .
N3 N 0.7249(5) 0.5444(4) 0.1844(19) 0.0295(19) Uani 1 1 d . U . . .
O1 O 0.8223(5) 0.4352(5) 0.2307(16) 0.055(3) Uani 1 1 d . U . . .
O2 O 0.7623(5) 0.3786(5) 0.0786(17) 0.061(3) Uani 1 1 d . U . . .
O3 O 0.6080(7) 0.4299(6) 0.006(2) 0.080(4) Uani 1 1 d . U . . .
O4 O 0.6611(5) 0.3512(5) 0.5680(16) 0.056(3) Uani 1 1 d . U . . .
O5 O 0.5948(6) 0.5295(6) 0.564(2) 0.082(5) Uani 1 1 d . U . . .
O6 O 0.9073(4) 0.5732(4) 0.8261(17) 0.050(3) Uani 1 1 d . U . . .
O7 O 0.7960(5) 0.6955(4) -0.0782(13) 0.041(2) Uani 1 1 d . U . . .
Re1 Re 0.69430(2) 0.46491(2) 0.33704(8) 0.03193(16) Uani 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 O3 1.127(18) . ?
C1 Re1 1.917(15) . ?
C2 O4 1.136(16) . ?
C2 Re1 1.933(14) . ?
C3 O5 1.154(17) . ?
C3 Re1 1.905(15) . ?
C4 N2 1.358(17) . ?
C4 C5 1.387(19) . ?
C4 H4 0.9300 . ?
C5 C6 1.353(19) . ?
C5 H5 0.9300 . ?
C6 O6 1.352(17) . ?
C6 C7 1.403(18) . ?
C7 C8 1.364(18) . ?
C7 H7 0.9300 . ?
C8 N2 1.355(16) . ?
C8 C9 1.480(18) . ?
C9 C10 1.358(17) . ?
C9 N3 1.360(17) . ?
C10 C11 1.398(19) . ?
C10 H10 0.9300 . ?
C11 O7 1.344(15) . ?
C11 C12 1.378(19) . ?
C12 C13 1.369(19) . ?
C12 H12 0.9300 . ?
C13 N3 1.37(2) . ?
C13 H13 0.9300 . ?
C14 O6 1.420(18) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.436(15) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N1 O2 1.184(15) . ?
N1 O1 1.257(15) . ?
N1 Re1 2.209(11) . ?
N2 Re1 2.158(11) . ?
N3 Re1 2.163(11) . ?

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
O3 C1 Re1 175.7(15) . . ?
O4 C2 Re1 176.9(14) . . ?
O5 C3 Re1 176.5(15) . . ?
N2 C4 C5 122.7(13) . . ?
N2 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C6 C5 C4 118.6(13) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
O6 C6 C5 123.9(13) . . ?
O6 C6 C7 116.0(13) . . ?
C5 C6 C7 120.0(14) . . ?
C8 C7 C6 118.5(13) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
N2 C8 C7 122.8(12) . . ?
N2 C8 C9 114.8(12) . . ?
C7 C8 C9 122.3(12) . . ?
C10 C9 N3 121.9(12) . . ?
C10 C9 C8 123.5(13) . . ?
N3 C9 C8 114.6(12) . . ?
C9 C10 C11 120.6(13) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
O7 C11 C12 125.6(12) . . ?
O7 C11 C10 116.6(12) . . ?
C12 C11 C10 117.7(12) . . ?
C13 C12 C11 119.8(13) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
N3 C13 C12 122.5(14) . . ?
N3 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 119.3(13) . . ?
O2 N1 Re1 121.7(10) . . ?
O1 N1 Re1 119.0(9) . . ?
C8 N2 C4 117.3(12) . . ?
C8 N2 Re1 118.0(9) . . ?
C4 N2 Re1 124.4(9) . . ?
C9 N3 C13 117.6(12) . . ?
C9 N3 Re1 117.9(9) . . ?
C13 N3 Re1 124.5(10) . . ?
C6 O6 C14 117.9(11) . . ?
C11 O7 C15 116.9(11) . . ?
C3 Re1 C1 90.2(7) . . ?
C3 Re1 C2 89.1(6) . . ?
C1 Re1 C2 89.7(6) . . ?
C3 Re1 N2 93.2(5) . . ?
C1 Re1 N2 169.5(5) . . ?
C2 Re1 N2 100.3(5) . . ?
C3 Re1 N3 93.2(5) . . ?
C1 Re1 N3 95.4(5) . . ?
C2 Re1 N3 174.4(6) . . ?
N2 Re1 N3 74.5(4) . . ?
C3 Re1 N1 176.7(6) . . ?
C1 Re1 N1 93.1(6) . . ?
C2 Re1 N1 91.4(5) . . ?
N2 Re1 N1 83.5(4) . . ?
N3 Re1 N1 86.1(4) . . ?

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
N2 C4 C5 C6 1(2) . . . . ?
C4 C5 C6 O6 -178.9(13) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
O6 C6 C7 C8 177.5(12) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C6 C7 C8 N2 2(2) . . . . ?
C6 C7 C8 C9 -178.8(12) . . . . ?
N2 C8 C9 C10 176.2(12) . . . . ?
C7 C8 C9 C10 -2.8(19) . . . . ?
N2 C8 C9 N3 -1.7(16) . . . . ?
C7 C8 C9 N3 179.3(12) . . . . ?
N3 C9 C10 C11 -2(2) . . . . ?
C8 C9 C10 C11 -179.3(12) . . . . ?
C9 C10 C11 O7 -177.4(12) . . . . ?
C9 C10 C11 C12 1.2(19) . . . . ?
O7 C11 C12 C13 178.7(13) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 N3 -1(2) . . . . ?
C7 C8 N2 C4 -2.0(19) . . . . ?
C9 C8 N2 C4 179.0(11) . . . . ?
C7 C8 N2 Re1 -176.3(10) . . . . ?
C9 C8 N2 Re1 4.8(14) . . . . ?
C5 C4 N2 C8 0.3(19) . . . . ?
C5 C4 N2 Re1 174.1(10) . . . . ?
C10 C9 N3 C13 0.5(19) . . . . ?
C8 C9 N3 C13 178.4(11) . . . . ?
C10 C9 N3 Re1 180.0(10) . . . . ?
C8 C9 N3 Re1 -2.1(14) . . . . ?
C12 C13 N3 C9 1(2) . . . . ?
C12 C13 N3 Re1 -178.4(10) . . . . ?
C5 C6 O6 C14 -4(2) . . . . ?
C7 C6 O6 C14 178.3(13) . . . . ?
C12 C11 O7 C15 5.9(19) . . . . ?
C10 C11 O7 C15 -175.6(12) . . . . ?

_refine_diff_density_max         1.465
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.131


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_220K
_database_code_depnum_ccdc_archive 'CCDC 1842790'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT973_VT_220K             
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 1.57 eA-3
RESPONSE: Slightly weak high angle data and so loss of resolution, partly due
to crystal irradiation in prior experiments, and partly due to increase in 
temperature. Reduced data resolution likely leads to truncation errors and 
spurious peaks in the region of the heavy atom.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.4172(8)
_cell_length_b                   22.4172(8)
_cell_length_c                   6.6766(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3355.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    2311
_cell_measurement_theta_min      3.6300
_cell_measurement_theta_max      26.6310

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0105
1 -1 0 0.0135
-1 1 0 0.0135
-1 1 -1 0.1144
1 -1 1 0.1144
-1 -1 0 0.0164
_exptl_absorpt_coefficient_mu    7.288
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6018
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.873
_diffrn_reflns_theta_max         25.656
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             3044
_reflns_number_gt                2643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_max     0.900
_reflns_Friedel_fraction_full    0.907

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0049P)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 973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3044
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0567
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.970
_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
C1 C 0.5581(5) 0.3608(6) 0.133(2) 0.035(3) Uani 1 1 d . U . . .
C2 C 0.6046(6) 0.3259(6) 0.484(2) 0.030(3) Uani 1 1 d . U . . .
C3 C 0.4944(6) 0.3682(6) 0.477(2) 0.036(3) Uani 1 1 d . U . . .
C4 C 0.5219(5) 0.2172(5) 0.6987(17) 0.030(3) Uani 1 1 d . U . . .
H4 H 0.5558 0.2374 0.7469 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5005(5) 0.1698(5) 0.8075(19) 0.032(3) Uani 1 1 d . U . . .
H5 H 0.5186 0.1581 0.9281 0.038 Uiso 1 1 calc R U . . .
C6 C 0.4518(6) 0.1404(6) 0.7342(18) 0.031(3) Uani 1 1 d . U . . .
C7 C 0.4252(6) 0.1587(5) 0.5594(17) 0.029(3) Uani 1 1 d . U . . .
H7 H 0.3913 0.1388 0.5105 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4485(5) 0.2060(5) 0.4575(16) 0.022(2) Uani 1 1 d . U . . .
C9 C 0.4241(5) 0.2288(5) 0.2667(16) 0.021(2) Uani 1 1 d . U . . .
C10 C 0.3739(5) 0.2059(5) 0.1763(19) 0.029(2) Uani 1 1 d . U . . .
H10 H 0.3536 0.1737 0.2356 0.034 Uiso 1 1 calc R U . . .
C11 C 0.3531(5) 0.2297(5) 0.0004(18) 0.026(2) Uani 1 1 d . U . . .
C12 C 0.3833(5) 0.2778(5) -0.0834(17) 0.028(3) Uani 1 1 d . U . . .
H12 H 0.3697 0.2956 -0.2024 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4338(5) 0.2986(5) 0.0134(18) 0.027(2) Uani 1 1 d . U . . .
H13 H 0.4544 0.3310 -0.0438 0.033 Uiso 1 1 calc R U . . .
C14 C 0.4518(6) 0.0721(6) 1.0107(19) 0.046(4) Uani 1 1 d . U . . .
H14A H 0.4545 0.1051 1.1043 0.068 Uiso 1 1 calc R U . . .
H14B H 0.4914 0.0565 0.9846 0.068 Uiso 1 1 calc R U . . .
H14C H 0.4270 0.0409 1.0675 0.068 Uiso 1 1 calc R U . . .
C15 C 0.2793(6) 0.2309(6) -0.2585(17) 0.033(3) Uani 1 1 d . U . . .
H15A H 0.2680 0.2718 -0.2298 0.049 Uiso 1 1 calc R U . . .
H15B H 0.2443 0.2085 -0.2992 0.049 Uiso 1 1 calc R U . . .
H15C H 0.3085 0.2303 -0.3656 0.049 Uiso 1 1 calc R U . . .
N1 N 0.5799(5) 0.2299(5) 0.1905(16) 0.033(2) Uani 1 1 d . U . . .
N2 N 0.4971(4) 0.2365(4) 0.5269(14) 0.0268(19) Uani 1 1 d . U . . .
N3 N 0.4552(4) 0.2753(4) 0.1847(16) 0.0242(18) Uani 1 1 d . U . . .
O1 O 0.5640(4) 0.1782(4) 0.2306(13) 0.051(3) Uani 1 1 d . U . . .
O2 O 0.6216(4) 0.2366(4) 0.0803(14) 0.053(3) Uani 1 1 d . U . . .
O3 O 0.5698(5) 0.3926(5) 0.0070(16) 0.065(3) Uani 1 1 d . U . . .
O4 O 0.6476(4) 0.3388(4) 0.5682(13) 0.046(3) Uani 1 1 d . U . . .
O5 O 0.4697(4) 0.4048(5) 0.5678(16) 0.064(3) Uani 1 1 d . U . . .
O6 O 0.4261(4) 0.0923(4) 0.8287(15) 0.044(2) Uani 1 1 d . U . . .
O7 O 0.3045(4) 0.2043(4) -0.0827(12) 0.037(2) Uani 1 1 d . U . . .
Re1 Re 0.53438(2) 0.30568(2) 0.33902(7) 0.02612(13) Uani 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 O3 1.134(15) . ?
C1 Re1 1.923(13) . ?
C2 O4 1.155(13) . ?
C2 Re1 1.902(13) . ?
C3 O5 1.160(14) . ?
C3 Re1 1.901(13) . ?
C4 N2 1.346(14) . ?
C4 C5 1.374(16) . ?
C4 H4 0.9400 . ?
C5 C6 1.366(16) . ?
C5 H5 0.9400 . ?
C6 C7 1.372(16) . ?
C6 O6 1.375(14) . ?
C7 C8 1.363(15) . ?
C7 H7 0.9400 . ?
C8 N2 1.368(13) . ?
C8 C9 1.478(15) . ?
C9 N3 1.367(14) . ?
C9 C10 1.377(15) . ?
C10 C11 1.371(16) . ?
C10 H10 0.9400 . ?
C11 O7 1.350(13) . ?
C11 C12 1.389(16) . ?
C12 C13 1.386(16) . ?
C12 H12 0.9400 . ?
C13 N3 1.346(17) . ?
C13 H13 0.9400 . ?
C14 O6 1.419(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 O7 1.431(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
N1 O2 1.199(12) . ?
N1 O1 1.243(13) . ?
N1 Re1 2.215(10) . ?
N2 Re1 2.163(10) . ?
N3 Re1 2.164(9) . ?

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
O3 C1 Re1 176.8(12) . . ?
O4 C2 Re1 178.5(12) . . ?
O5 C3 Re1 177.2(13) . . ?
N2 C4 C5 123.6(12) . . ?
N2 C4 H4 118.2 . . ?
C5 C4 H4 118.2 . . ?
C6 C5 C4 117.6(12) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
C5 C6 C7 120.4(13) . . ?
C5 C6 O6 123.3(11) . . ?
C7 C6 O6 116.3(12) . . ?
C8 C7 C6 119.4(12) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 N2 121.6(11) . . ?
C7 C8 C9 124.0(11) . . ?
N2 C8 C9 114.4(10) . . ?
N3 C9 C10 121.7(10) . . ?
N3 C9 C8 114.9(11) . . ?
C10 C9 C8 123.4(11) . . ?
C11 C10 C9 120.5(11) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O7 C11 C10 117.5(10) . . ?
O7 C11 C12 123.6(11) . . ?
C10 C11 C12 118.9(11) . . ?
C13 C12 C11 118.1(11) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
N3 C13 C12 123.8(12) . . ?
N3 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 118.1(11) . . ?
O2 N1 Re1 122.6(9) . . ?
O1 N1 Re1 119.2(9) . . ?
C4 N2 C8 117.3(10) . . ?
C4 N2 Re1 124.4(8) . . ?
C8 N2 Re1 118.0(7) . . ?
C13 N3 C9 117.1(10) . . ?
C13 N3 Re1 125.0(9) . . ?
C9 N3 Re1 117.9(8) . . ?
C6 O6 C14 118.2(10) . . ?
C11 O7 C15 118.7(9) . . ?
C3 Re1 C2 88.2(5) . . ?
C3 Re1 C1 90.2(6) . . ?
C2 Re1 C1 88.9(5) . . ?
C3 Re1 N2 93.7(5) . . ?
C2 Re1 N2 101.3(5) . . ?
C1 Re1 N2 169.2(5) . . ?
C3 Re1 N3 94.4(5) . . ?
C2 Re1 N3 175.2(5) . . ?
C1 Re1 N3 95.1(5) . . ?
N2 Re1 N3 74.5(4) . . ?
C3 Re1 N1 177.2(5) . . ?
C2 Re1 N1 91.7(5) . . ?
C1 Re1 N1 92.6(5) . . ?
N2 Re1 N1 83.6(4) . . ?
N3 Re1 N1 85.6(4) . . ?

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
N2 C4 C5 C6 1.0(19) . . . . ?
C4 C5 C6 C7 -1.0(19) . . . . ?
C4 C5 C6 O6 -180.0(12) . . . . ?
C5 C6 C7 C8 1.2(19) . . . . ?
O6 C6 C7 C8 -179.8(12) . . . . ?
C6 C7 C8 N2 -1.3(18) . . . . ?
C6 C7 C8 C9 179.0(11) . . . . ?
C7 C8 C9 N3 -177.8(11) . . . . ?
N2 C8 C9 N3 2.5(14) . . . . ?
C7 C8 C9 C10 2.6(18) . . . . ?
N2 C8 C9 C10 -177.2(11) . . . . ?
N3 C9 C10 C11 -0.6(18) . . . . ?
C8 C9 C10 C11 179.1(11) . . . . ?
C9 C10 C11 O7 178.6(10) . . . . ?
C9 C10 C11 C12 -0.8(18) . . . . ?
O7 C11 C12 C13 -178.0(11) . . . . ?
C10 C11 C12 C13 1.3(17) . . . . ?
C11 C12 C13 N3 -0.5(18) . . . . ?
C5 C4 N2 C8 -1.1(18) . . . . ?
C5 C4 N2 Re1 -174.2(9) . . . . ?
C7 C8 N2 C4 1.2(17) . . . . ?
C9 C8 N2 C4 -179.0(10) . . . . ?
C7 C8 N2 Re1 174.8(9) . . . . ?
C9 C8 N2 Re1 -5.5(12) . . . . ?
C12 C13 N3 C9 -0.8(18) . . . . ?
C12 C13 N3 Re1 179.2(8) . . . . ?
C10 C9 N3 C13 1.4(17) . . . . ?
C8 C9 N3 C13 -178.3(10) . . . . ?
C10 C9 N3 Re1 -178.7(8) . . . . ?
C8 C9 N3 Re1 1.6(13) . . . . ?
C5 C6 O6 C14 -1(2) . . . . ?
C7 C6 O6 C14 -179.6(11) . . . . ?
C10 C11 O7 C15 175.6(11) . . . . ?
C12 C11 O7 C15 -5.1(17) . . . . ?

_refine_diff_density_max         1.007
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.142


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_175K
_database_code_depnum_ccdc_archive 'CCDC 1842778'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT342_PSS_175K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02111 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.83 A)
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.739(2)
_cell_length_b                   22.739(2)
_cell_length_c                   6.5506(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3387.2(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    2493
_cell_measurement_theta_min      3.2320
_cell_measurement_theta_max      30.7050

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
-1 -1 -1 0.1206
1 1 1 0.1391
-1 1 0 0.0116
1 1 0 0.0096
-1 -1 0 0.0096
_exptl_absorpt_coefficient_mu    7.219
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6047
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.236
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.934
_reflns_number_total             2900
_reflns_number_gt                2498
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_max     0.855
_reflns_Friedel_fraction_full    0.860

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0368P)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 885 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2900
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.0966
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4014(7) 0.8228(7) 0.248(2) 0.024(3) Uani 1 1 d . U . . .
C2 C 0.4475(7) 0.8597(7) 0.611(3) 0.034(3) Uani 1 1 d . U . . .
C3 C 0.5082(8) 0.8680(8) 0.259(2) 0.029(3) Uani 1 1 d . U . . .
C4 C 0.5723(7) 0.8027(8) 0.729(2) 0.027(3) Uani 1 1 d . U . . .
H4 H 0.5532 0.8359 0.7788 0.033 Uiso 1 1 calc R U . . .
C5 C 0.6207(7) 0.7810(7) 0.833(2) 0.026(3) Uani 1 1 d . U . . .
H5 H 0.6339 0.7990 0.9515 0.031 Uiso 1 1 calc R U . . .
C6 C 0.6489(7) 0.7317(7) 0.755(2) 0.023(3) Uani 1 1 d . U . . .
C7 C 0.6287(6) 0.7063(7) 0.577(2) 0.024(3) Uani 1 1 d . U . . .
H7 H 0.6477 0.6735 0.5233 0.029 Uiso 1 1 calc R U . . .
C8 C 0.5804(7) 0.7296(7) 0.479(2) 0.021(3) Uani 1 1 d . U . . .
C9 C 0.5557(7) 0.7063(7) 0.287(2) 0.025(3) Uani 1 1 d . U . . .
C10 C 0.5797(8) 0.6585(8) 0.190(3) 0.029(3) Uani 1 1 d . U . . .
H10 H 0.6121 0.6393 0.2455 0.035 Uiso 1 1 calc R U . . .
C11 C 0.5547(8) 0.6391(8) 0.007(3) 0.029(3) Uani 1 1 d . U . . .
C12 C 0.5073(7) 0.6688(7) -0.069(2) 0.027(3) Uani 1 1 d . U . . .
H12 H 0.4896 0.6569 -0.1903 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4864(8) 0.7163(7) 0.036(2) 0.028(3) Uani 1 1 d . U . . .
H13 H 0.4537 0.7358 -0.0166 0.033 Uiso 1 1 calc R U . . .
C14 C 0.7190(8) 0.7317(9) 1.028(3) 0.041(5) Uani 1 1 d . U . . .
H14A H 0.7344 0.7699 0.9960 0.061 Uiso 1 1 calc R U . . .
H14B H 0.7498 0.7076 1.0834 0.061 Uiso 1 1 calc R U . . .
H14C H 0.6880 0.7354 1.1266 0.061 Uiso 1 1 calc R U . . .
C15 C 0.5542(10) 0.5695(9) -0.268(3) 0.056(6) Uani 1 1 d . U . . .
H15A H 0.5599 0.5983 -0.3729 0.083 Uiso 1 1 calc R U . . .
H15B H 0.5129 0.5626 -0.2497 0.083 Uiso 1 1 calc R U . . .
H15C H 0.5732 0.5335 -0.3063 0.083 Uiso 1 1 calc R U . . .
N2 N 0.5519(6) 0.7774(6) 0.5576(18) 0.023(2) Uani 1 1 d . U . . .
N3 N 0.5102(6) 0.7367(6) 0.2101(19) 0.026(2) Uani 1 1 d . U . . .
O3 O 0.3580(5) 0.8345(5) 0.1693(19) 0.044(3) Uani 1 1 d . U . . .
O4 O 0.4344(6) 0.8913(6) 0.7329(19) 0.052(4) Uani 1 1 d . U . . .
O5 O 0.5323(6) 0.9050(6) 0.170(2) 0.054(4) Uani 1 1 d . U . . .
O6 O 0.6960(5) 0.7045(5) 0.8430(15) 0.032(3) Uani 1 1 d . U . . .
O7 O 0.5792(6) 0.5908(5) -0.0784(19) 0.045(3) Uani 1 1 d . U . . .
Re1 Re 0.47228(3) 0.80535(3) 0.39819(9) 0.02549(19) Uani 1 1 d . U . . .
N1 N 0.4256(17) 0.7250(12) 0.554(8) 0.035(2) Uani 0.345(16) 1 d D U P A 1
O1 O 0.4406(14) 0.6763(13) 0.506(5) 0.035(2) Uani 0.345(16) 1 d D U P A 1
O2 O 0.3835(15) 0.7343(14) 0.658(6) 0.035(2) Uani 0.345(16) 1 d D U P A 1
N1A N 0.3962(8) 0.7163(7) 0.631(4) 0.035(2) Uani 0.655(16) 1 d D U P A 2
O1A O 0.4432(7) 0.7275(8) 0.533(3) 0.035(2) Uani 0.655(16) 1 d D U P A 2
O2A O 0.3645(7) 0.7632(7) 0.650(3) 0.035(2) Uani 0.655(16) 1 d D U P A 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
C1 O3 1.144(18) . ?
C1 Re1 1.930(16) . ?
C2 O4 1.117(19) . ?
C2 Re1 1.943(18) . ?
C3 O5 1.158(19) . ?
C3 Re1 1.880(17) . ?
C4 N2 1.34(2) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.39(2) . ?
C5 H5 0.9300 . ?
C6 O6 1.366(18) . ?
C6 C7 1.38(2) . ?
C7 C8 1.38(2) . ?
C7 H7 0.9300 . ?
C8 N2 1.36(2) . ?
C8 C9 1.48(2) . ?
C9 N3 1.342(19) . ?
C9 C10 1.37(2) . ?
C10 C11 1.40(2) . ?
C10 H10 0.9300 . ?
C11 O7 1.35(2) . ?
C11 C12 1.37(2) . ?
C12 C13 1.37(2) . ?
C12 H12 0.9300 . ?
C13 N3 1.347(19) . ?
C13 H13 0.9300 . ?
C14 O6 1.458(18) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.45(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 Re1 2.185(13) . ?
N3 Re1 2.167(13) . ?
Re1 O1A 2.086(18) . ?
Re1 N1 2.35(3) . ?
N1 O2 1.194(13) . ?
N1 O1 1.199(14) . ?
N1A O1A 1.274(12) . ?
N1A O2A 1.292(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
O3 C1 Re1 175.7(14) . . ?
O4 C2 Re1 178.6(16) . . ?
O5 C3 Re1 177.2(16) . . ?
N2 C4 C5 122.1(15) . . ?
N2 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 118.3(14) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
O6 C6 C7 115.4(14) . . ?
O6 C6 C5 125.0(13) . . ?
C7 C6 C5 119.6(15) . . ?
C6 C7 C8 119.8(15) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
N2 C8 C7 120.6(14) . . ?
N2 C8 C9 115.3(14) . . ?
C7 C8 C9 124.2(15) . . ?
N3 C9 C10 122.9(15) . . ?
N3 C9 C8 115.3(14) . . ?
C10 C9 C8 121.8(15) . . ?
C9 C10 C11 119.0(17) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
O7 C11 C12 125.1(15) . . ?
O7 C11 C10 116.4(16) . . ?
C12 C11 C10 118.5(17) . . ?
C13 C12 C11 118.9(15) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N3 C13 C12 124.0(16) . . ?
N3 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 119.5(14) . . ?
C4 N2 Re1 124.0(11) . . ?
C8 N2 Re1 116.4(10) . . ?
C9 N3 C13 116.7(14) . . ?
C9 N3 Re1 117.7(10) . . ?
C13 N3 Re1 124.8(11) . . ?
C6 O6 C14 116.1(13) . . ?
C11 O7 C15 117.7(14) . . ?
C3 Re1 C1 87.6(7) . . ?
C3 Re1 C2 89.6(7) . . ?
C1 Re1 C2 89.6(7) . . ?
C3 Re1 O1A 170.7(7) . . ?
C1 Re1 O1A 97.3(7) . . ?
C2 Re1 O1A 98.3(7) . . ?
C3 Re1 N3 95.5(6) . . ?
C1 Re1 N3 100.9(6) . . ?
C2 Re1 N3 168.4(6) . . ?
O1A Re1 N3 75.9(6) . . ?
C3 Re1 N2 95.3(6) . . ?
C1 Re1 N2 174.7(6) . . ?
C2 Re1 N2 94.8(6) . . ?
O1A Re1 N2 79.2(7) . . ?
N3 Re1 N2 74.5(5) . . ?
C3 Re1 N1 176.6(14) . . ?
C1 Re1 N1 90.3(14) . . ?
C2 Re1 N1 93.0(10) . . ?
N3 Re1 N1 82.3(8) . . ?
N2 Re1 N1 86.6(13) . . ?
O2 N1 O1 123(2) . . ?
O2 N1 Re1 118(2) . . ?
O1 N1 Re1 118(2) . . ?
O1A N1A O2A 110.6(13) . . ?
N1A O1A Re1 130.5(12) . . ?

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
N2 C4 C5 C6 1(2) . . . . ?
C4 C5 C6 O6 -178.2(14) . . . . ?
C4 C5 C6 C7 1(2) . . . . ?
O6 C6 C7 C8 178.4(13) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C6 C7 C8 N2 -1(2) . . . . ?
C6 C7 C8 C9 179.1(14) . . . . ?
N2 C8 C9 N3 3(2) . . . . ?
C7 C8 C9 N3 -177.1(14) . . . . ?
N2 C8 C9 C10 -179.9(16) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
N3 C9 C10 C11 -2(3) . . . . ?
C8 C9 C10 C11 -179.3(14) . . . . ?
C9 C10 C11 O7 -178.3(16) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
O7 C11 C12 C13 178.6(16) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 N3 1(2) . . . . ?
C5 C4 N2 C8 -2(2) . . . . ?
C5 C4 N2 Re1 175.4(11) . . . . ?
C7 C8 N2 C4 2(2) . . . . ?
C9 C8 N2 C4 -177.9(13) . . . . ?
C7 C8 N2 Re1 -175.6(11) . . . . ?
C9 C8 N2 Re1 4.6(17) . . . . ?
C10 C9 N3 C13 3(2) . . . . ?
C8 C9 N3 C13 -179.5(13) . . . . ?
C10 C9 N3 Re1 173.8(13) . . . . ?
C8 C9 N3 Re1 -8.9(18) . . . . ?
C12 C13 N3 C9 -3(2) . . . . ?
C12 C13 N3 Re1 -172.5(12) . . . . ?
C7 C6 O6 C14 178.3(14) . . . . ?
C5 C6 O6 C14 -3(2) . . . . ?
C12 C11 O7 C15 1(3) . . . . ?
C10 C11 O7 C15 179.9(16) . . . . ?
O2A N1A O1A Re1 -3(3) . . . . ?

_refine_diff_density_max         1.106
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.166


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_GS_170K
_database_code_depnum_ccdc_archive 'CCDC 1842782'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.3068(3)
_cell_length_b                   22.3068(3)
_cell_length_c                   6.6532(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3310.59(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    4824
_cell_measurement_theta_min      3.1920
_cell_measurement_theta_max      28.7660

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0093
1 -1 0 0.0091
-1 1 0 0.0100
0 0 -1 0.1246
0 0 1 0.1246
-1 -1 0 0.0123
_exptl_absorpt_coefficient_mu    7.386
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            10308
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.888
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3365
_reflns_number_gt                3092
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_max     0.975
_reflns_Friedel_fraction_full    0.983

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0093P)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 1260 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3365
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0428
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.972
_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
C1 C 0.8607(3) 0.4409(3) 0.6180(13) 0.0247(17) Uani 1 1 d . U . . .
C2 C 0.8262(4) 0.3938(3) 0.2630(12) 0.0216(16) Uani 1 1 d . U . . .
C3 C 0.8694(4) 0.5065(4) 0.2720(13) 0.0260(18) Uani 1 1 d . U . . .
C4 C 0.7175(3) 0.4779(3) 0.0499(11) 0.0213(16) Uani 1 1 d . U . . .
H4 H 0.7384 0.4440 -0.0011 0.026 Uiso 1 1 calc R U . . .
C5 C 0.6696(3) 0.4990(3) -0.0573(12) 0.0213(15) Uani 1 1 d . U . . .
H5 H 0.6575 0.4797 -0.1781 0.026 Uiso 1 1 calc R U . . .
C6 C 0.6393(4) 0.5485(4) 0.0123(11) 0.0229(17) Uani 1 1 d . U . . .
C7 C 0.6592(4) 0.5753(4) 0.1885(11) 0.0207(16) Uani 1 1 d . U . . .
H7 H 0.6400 0.6104 0.2381 0.025 Uiso 1 1 calc R U . . .
C8 C 0.7069(3) 0.5508(3) 0.2910(11) 0.0169(14) Uani 1 1 d . U . . .
C9 C 0.7291(3) 0.5755(3) 0.4842(10) 0.0160(14) Uani 1 1 d . U . . .
C10 C 0.7059(3) 0.6263(3) 0.5731(12) 0.0183(14) Uani 1 1 d . U . . .
H10 H 0.6738 0.6474 0.5116 0.022 Uiso 1 1 calc R U . . .
C11 C 0.7300(3) 0.6464(3) 0.7531(11) 0.0170(14) Uani 1 1 d . U . . .
C12 C 0.7782(3) 0.6158(3) 0.8364(11) 0.0207(16) Uani 1 1 d . U . . .
H12 H 0.7966 0.6292 0.9572 0.025 Uiso 1 1 calc R U . . .
C13 C 0.7985(3) 0.5657(3) 0.7387(12) 0.0231(16) Uani 1 1 d . U . . .
H13 H 0.8312 0.5445 0.7961 0.028 Uiso 1 1 calc R U . . .
C14 C 0.5716(4) 0.5482(4) -0.2622(12) 0.032(2) Uani 1 1 d . U . . .
H14A H 0.6043 0.5482 -0.3605 0.048 Uiso 1 1 calc R U . . .
H14B H 0.5379 0.5717 -0.3145 0.048 Uiso 1 1 calc R U . . .
H14C H 0.5585 0.5069 -0.2379 0.048 Uiso 1 1 calc R U . . .
C15 C 0.7310(4) 0.7214(4) 1.0102(11) 0.028(2) Uani 1 1 d . U . . .
H15A H 0.7730 0.7315 0.9836 0.042 Uiso 1 1 calc R U . . .
H15B H 0.7289 0.6921 1.1197 0.042 Uiso 1 1 calc R U . . .
H15C H 0.7091 0.7578 1.0486 0.042 Uiso 1 1 calc R U . . .
N1 N 0.7294(3) 0.4190(3) 0.5565(9) 0.0218(13) Uani 1 1 d . U . . .
N2 N 0.7366(3) 0.5020(3) 0.2228(9) 0.0186(12) Uani 1 1 d . U . . .
N3 N 0.7751(3) 0.5448(3) 0.5673(11) 0.0189(12) Uani 1 1 d . U . . .
O1 O 0.6770(3) 0.4355(3) 0.5182(8) 0.0321(14) Uani 1 1 d . U . . .
O2 O 0.7372(3) 0.3780(3) 0.6731(8) 0.0404(16) Uani 1 1 d . U . . .
O3 O 0.8927(3) 0.4298(3) 0.7472(10) 0.0508(18) Uani 1 1 d . U . . .
O4 O 0.8392(3) 0.3510(3) 0.1788(8) 0.0338(15) Uani 1 1 d . U . . .
O5 O 0.9061(3) 0.5300(3) 0.1825(10) 0.0472(19) Uani 1 1 d . U . . .
O6 O 0.5920(2) 0.5739(2) -0.0790(9) 0.0312(13) Uani 1 1 d . U . . .
O7 O 0.7046(2) 0.6963(2) 0.8321(7) 0.0246(13) Uani 1 1 d . U . . .
Re1 Re 0.80587(2) 0.46500(2) 0.41141(4) 0.01863(9) Uani 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 O3 1.143(9) . ?
C1 Re1 1.917(8) . ?
C2 O4 1.144(9) . ?
C2 Re1 1.925(8) . ?
C3 O5 1.140(9) . ?
C3 Re1 1.930(8) . ?
C4 N2 1.340(9) . ?
C4 C5 1.367(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(11) . ?
C5 H5 0.9500 . ?
C6 O6 1.342(9) . ?
C6 C7 1.389(10) . ?
C7 C8 1.378(10) . ?
C7 H7 0.9500 . ?
C8 N2 1.353(9) . ?
C8 C9 1.483(10) . ?
C9 N3 1.351(9) . ?
C9 C10 1.379(10) . ?
C10 C11 1.387(10) . ?
C10 H10 0.9500 . ?
C11 O7 1.355(8) . ?
C11 C12 1.389(10) . ?
C12 C13 1.370(10) . ?
C12 H12 0.9500 . ?
C13 N3 1.338(11) . ?
C13 H13 0.9500 . ?
C14 O6 1.423(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.438(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1 O2 1.212(8) . ?
N1 O1 1.250(8) . ?
N1 Re1 2.213(6) . ?
N2 Re1 2.155(6) . ?
N3 Re1 2.172(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
O3 C1 Re1 175.7(7) . . ?
O4 C2 Re1 178.2(8) . . ?
O5 C3 Re1 177.2(8) . . ?
N2 C4 C5 123.9(7) . . ?
N2 C4 H4 118.0 . . ?
C5 C4 H4 118.0 . . ?
C4 C5 C6 119.0(7) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
O6 C6 C5 125.0(7) . . ?
O6 C6 C7 116.8(7) . . ?
C5 C6 C7 118.2(8) . . ?
C8 C7 C6 119.6(8) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N2 C8 C7 122.1(7) . . ?
N2 C8 C9 115.2(6) . . ?
C7 C8 C9 122.7(7) . . ?
N3 C9 C10 121.7(7) . . ?
N3 C9 C8 114.8(7) . . ?
C10 C9 C8 123.5(7) . . ?
C9 C10 C11 119.4(7) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
O7 C11 C10 115.9(6) . . ?
O7 C11 C12 124.9(7) . . ?
C10 C11 C12 119.1(7) . . ?
C13 C12 C11 117.8(7) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
N3 C13 C12 124.0(8) . . ?
N3 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 119.2(7) . . ?
O2 N1 Re1 121.1(5) . . ?
O1 N1 Re1 119.6(5) . . ?
C4 N2 C8 117.1(6) . . ?
C4 N2 Re1 125.0(5) . . ?
C8 N2 Re1 117.6(5) . . ?
C13 N3 C9 118.0(7) . . ?
C13 N3 Re1 124.6(5) . . ?
C9 N3 Re1 117.4(5) . . ?
C6 O6 C14 118.0(6) . . ?
C11 O7 C15 117.9(6) . . ?
C1 Re1 C2 89.2(3) . . ?
C1 Re1 C3 90.6(4) . . ?
C2 Re1 C3 88.6(3) . . ?
C1 Re1 N2 169.3(3) . . ?
C2 Re1 N2 100.7(3) . . ?
C3 Re1 N2 93.6(3) . . ?
C1 Re1 N3 95.2(3) . . ?
C2 Re1 N3 174.9(3) . . ?
C3 Re1 N3 93.9(3) . . ?
N2 Re1 N3 74.8(2) . . ?
C1 Re1 N1 92.8(3) . . ?
C2 Re1 N1 91.3(3) . . ?
C3 Re1 N1 176.6(3) . . ?
N2 Re1 N1 83.0(2) . . ?
N3 Re1 N1 85.8(2) . . ?

_refine_diff_density_max         0.649
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.107


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_250K
_database_code_depnum_ccdc_archive 'CCDC 1842785'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_THETM01_PSS_250K            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data = no data above
0.9 A resolution.
;
_vrf_PLAT090_PSS_250K            
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.57 Note
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
leading to overall loss of unique reflection data.
;
_vrf_PLAT342_PSS_250K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.05111 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
;
_vrf_PLAT973_PSS_250K            
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 1.93 eA-3
RESPONSE: ...
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.358(2)
_cell_length_b                   22.358(2)
_cell_length_c                   6.6738(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3336.1(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    1257
_cell_measurement_theta_min      3.6360
_cell_measurement_theta_max      26.4610

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
-1 1 1 0.1206
1 -1 -1 0.1391
-1 1 0 0.0116
0 -1 0 0.0096
0 1 0 0.0096
_exptl_absorpt_coefficient_mu    7.330
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6308
_diffrn_reflns_av_unetI/netI     0.1219
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.881
_diffrn_reflns_theta_max         23.238
_diffrn_reflns_theta_full        23.238
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2386
_reflns_number_gt                1977
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.990

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0754P)²+91.8762P] 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 592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2386
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0786
_refine_ls_wR_factor_ref         0.1811
_refine_ls_wR_factor_gt          0.1671
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6402(15) 0.5597(14) 0.864(6) 0.038(4) Uani 1 1 d . U . . .
C2 C 0.6720(15) 0.6056(15) 0.513(6) 0.038(4) Uani 1 1 d . U . . .
C3 C 0.6330(16) 0.4909(15) 0.533(6) 0.038(4) Uani 1 1 d . U . . .
C4 C 0.7839(15) 0.5221(15) 0.300(5) 0.039(7) Uani 1 1 d . U . . .
H4 H 0.7640 0.5554 0.2500 0.047 Uiso 1 1 calc R U . . .
C5 C 0.8312(14) 0.5018(15) 0.191(6) 0.037(7) Uani 1 1 d . U . . .
H5 H 0.8441 0.5210 0.0756 0.045 Uiso 1 1 calc R U . . .
C6 C 0.8594(16) 0.4504(16) 0.264(6) 0.039(7) Uani 1 1 d . U . . .
C7 C 0.8414(17) 0.4249(17) 0.440(6) 0.044(9) Uani 1 1 d . U . . .
H7 H 0.8609 0.3912 0.4895 0.053 Uiso 1 1 calc R U . . .
C8 C 0.7937(14) 0.4498(14) 0.544(5) 0.030(6) Uani 1 1 d . U . . .
C9 C 0.7710(15) 0.4239(15) 0.732(5) 0.033(6) Uani 1 1 d . U . . .
C10 C 0.7942(14) 0.3735(14) 0.820(6) 0.034(6) Uani 1 1 d . U . . .
H10 H 0.8261 0.3534 0.7607 0.041 Uiso 1 1 calc R U . . .
C11 C 0.7696(15) 0.3531(14) 0.996(6) 0.034(6) Uani 1 1 d . U . . .
C12 C 0.7218(15) 0.3843(15) 1.081(6) 0.039(7) Uani 1 1 d . U . . .
H12 H 0.7046 0.3706 1.1996 0.046 Uiso 1 1 calc R U . . .
C13 C 0.7004(15) 0.4338(15) 0.994(6) 0.037(7) Uani 1 1 d . U . . .
H13 H 0.6692 0.4548 1.0535 0.045 Uiso 1 1 calc R U . . .
C14 C 0.9263(18) 0.4523(19) -0.005(6) 0.059(11) Uani 1 1 d . U . . .
H14A H 0.8949 0.4482 -0.1024 0.088 Uiso 1 1 calc R U . . .
H14B H 0.9615 0.4321 -0.0528 0.088 Uiso 1 1 calc R U . . .
H14C H 0.9351 0.4939 0.0141 0.088 Uiso 1 1 calc R U . . .
C15 C 0.7702(15) 0.2798(15) 1.255(5) 0.037(7) Uani 1 1 d . U . . .
H15A H 0.7300 0.2673 1.2261 0.055 Uiso 1 1 calc R U . . .
H15B H 0.7696 0.3094 1.3589 0.055 Uiso 1 1 calc R U . . .
H15C H 0.7933 0.2460 1.2977 0.055 Uiso 1 1 calc R U . . .
N1 N 0.7707(12) 0.5793(12) 0.808(5) 0.038(4) Uani 1 1 d . U . . .
N2 N 0.7628(11) 0.4981(11) 0.474(4) 0.031(3) Uani 1 1 d . U . . .
N3 N 0.7250(12) 0.4543(11) 0.812(5) 0.033(3) Uani 1 1 d . U . . .
O1 O 0.8227(12) 0.5641(13) 0.767(4) 0.060(7) Uani 1 1 d . U . . .
O2 O 0.7628(13) 0.6211(12) 0.923(4) 0.061(7) Uani 1 1 d . U . . .
O3 O 0.6066(16) 0.5699(13) 0.994(6) 0.089(11) Uani 1 1 d . U . . .
O4 O 0.6623(13) 0.6491(12) 0.428(4) 0.064(9) Uani 1 1 d . U . . .
O5 O 0.5951(14) 0.4699(14) 0.434(5) 0.081(11) Uani 1 1 d . U . . .
O6 O 0.9082(11) 0.4270(11) 0.177(4) 0.052(6) Uani 1 1 d . U . . .
O7 O 0.7965(11) 0.3049(11) 1.077(4) 0.045(6) Uani 1 1 d . U . . .
Re1 Re 0.69437(6) 0.53453(6) 0.6618(2) 0.0359(5) Uani 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 O3 1.17(4) . ?
C1 Re1 1.90(4) . ?
C2 O4 1.15(4) . ?
C2 Re1 1.94(4) . ?
C3 O5 1.17(4) . ?
C3 Re1 1.89(4) . ?
C4 C5 1.36(5) . ?
C4 N2 1.37(4) . ?
C5 C6 1.40(5) . ?
C6 O6 1.34(4) . ?
C6 C7 1.37(5) . ?
C7 C8 1.39(5) . ?
C8 N2 1.36(4) . ?
C8 C9 1.47(5) . ?
C9 N3 1.34(4) . ?
C9 C10 1.37(4) . ?
C10 C11 1.38(5) . ?
C11 O7 1.35(4) . ?
C11 C12 1.40(5) . ?
C12 C13 1.34(5) . ?
C13 N3 1.41(5) . ?
C14 O6 1.40(5) . ?
C15 O7 1.44(4) . ?
N1 O2 1.22(4) . ?
N1 O1 1.24(4) . ?
N1 Re1 2.21(3) . ?
N2 Re1 2.14(3) . ?
N3 Re1 2.16(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
O3 C1 Re1 174(3) . . ?
O4 C2 Re1 176(3) . . ?
O5 C3 Re1 171(3) . . ?
C5 C4 N2 126(3) . . ?
C4 C5 C6 116(3) . . ?
O6 C6 C7 117(3) . . ?
O6 C6 C5 122(3) . . ?
C7 C6 C5 121(4) . . ?
C6 C7 C8 119(3) . . ?
N2 C8 C7 122(3) . . ?
N2 C8 C9 115(3) . . ?
C7 C8 C9 122(3) . . ?
N3 C9 C10 122(3) . . ?
N3 C9 C8 114(3) . . ?
C10 C9 C8 124(3) . . ?
C9 C10 C11 119(3) . . ?
O7 C11 C10 115(3) . . ?
O7 C11 C12 125(3) . . ?
C10 C11 C12 119(3) . . ?
C13 C12 C11 121(3) . . ?
C12 C13 N3 120(3) . . ?
O2 N1 O1 119(3) . . ?
O2 N1 Re1 121(2) . . ?
O1 N1 Re1 120(2) . . ?
C8 N2 C4 115(3) . . ?
C8 N2 Re1 118(2) . . ?
C4 N2 Re1 127(2) . . ?
C9 N3 C13 118(3) . . ?
C9 N3 Re1 119(2) . . ?
C13 N3 Re1 123(2) . . ?
C6 O6 C14 117(3) . . ?
C11 O7 C15 117(3) . . ?
C3 Re1 C1 90.8(16) . . ?
C3 Re1 C2 90.2(14) . . ?
C1 Re1 C2 87.5(16) . . ?
C3 Re1 N2 93.2(13) . . ?
C1 Re1 N2 170.2(13) . . ?
C2 Re1 N2 101.4(13) . . ?
C3 Re1 N3 90.7(13) . . ?
C1 Re1 N3 96.8(13) . . ?
C2 Re1 N3 175.6(14) . . ?
N2 Re1 N3 74.2(11) . . ?
C3 Re1 N1 175.4(13) . . ?
C1 Re1 N1 92.4(13) . . ?
C2 Re1 N1 93.1(13) . . ?
N2 Re1 N1 83.0(11) . . ?
N3 Re1 N1 85.8(10) . . ?

_refine_diff_density_max         1.884
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.202


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_220K
_database_code_depnum_ccdc_archive 'CCDC 1842783'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_THETM01_PSS_220K            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data = no data above
0.9 A resolution.
;
_vrf_PLAT973_PSS_220K            
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 2.51 eA-3
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
_vrf_PLAT090_PSS_220K            
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.67 Note
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
leading to overall loss of unique reflection data.
;
_vrf_PLAT342_PSS_220K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06667 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.543(2)
_cell_length_b                   22.543(2)
_cell_length_c                   6.6249(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3366.7(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    1091
_cell_measurement_theta_min      3.5960
_cell_measurement_theta_max      29.5520

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.022
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0110
-1 -1 0 0.0214
1 1 0 0.0116
2 1 -2 0.1260
1 -1 1 0.1515
-1 2 -1 0.1131
1 -1 0 0.0110
_exptl_absorpt_coefficient_mu    7.263
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6256
_diffrn_reflns_av_unetI/netI     0.1762
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.857
_diffrn_reflns_theta_max         23.254
_diffrn_reflns_theta_full        23.254
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2412
_reflns_number_gt                1772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0888P)²+172.9096P] 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 369 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2412
_refine_ls_number_parameters     235
_refine_ls_number_restraints     265
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.1062
_refine_ls_wR_factor_ref         0.2401
_refine_ls_wR_factor_gt          0.2114
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5571(19) 0.6423(19) 0.150(9) 0.043(4) Uani 1 1 d . U . . .
C2 C 0.601(2) 0.676(2) 0.480(8) 0.043(4) Uani 1 1 d . U . . .
C3 C 0.491(2) 0.635(2) 0.482(8) 0.044(5) Uani 1 1 d . U . . .
C4 C 0.517(2) 0.784(2) 0.703(8) 0.048(10) Uani 1 1 d . U . . .
H4 H 0.5497 0.7636 0.7518 0.058 Uiso 1 1 calc R U . . .
C5 C 0.497(2) 0.8304(19) 0.821(8) 0.045(9) Uani 1 1 d . U . . .
H5 H 0.5155 0.8412 0.9419 0.054 Uiso 1 1 calc R U . . .
C6 C 0.449(2) 0.859(2) 0.743(8) 0.040(9) Uani 1 1 d . U . . .
C7 C 0.424(2) 0.843(2) 0.558(7) 0.042(10) Uani 1 1 d . U . . .
H7 H 0.3933 0.8655 0.4992 0.051 Uiso 1 1 calc R U . . .
C8 C 0.4455(19) 0.7922(19) 0.465(7) 0.035(7) Uani 1 1 d . U . . .
C9 C 0.422(2) 0.770(2) 0.268(7) 0.042(9) Uani 1 1 d . U . . .
C10 C 0.3716(18) 0.7943(19) 0.177(7) 0.036(8) Uani 1 1 d . U . . .
H10 H 0.3517 0.8265 0.2325 0.043 Uiso 1 1 calc R U . . .
C11 C 0.353(2) 0.769(2) 0.005(8) 0.043(9) Uani 1 1 d . U . . .
C12 C 0.381(2) 0.722(2) -0.083(7) 0.046(10) Uani 1 1 d . U . . .
H12 H 0.3677 0.7059 -0.2036 0.055 Uiso 1 1 calc R U . . .
C13 C 0.430(2) 0.700(2) 0.010(8) 0.045(10) Uani 1 1 d . U . . .
H13 H 0.4491 0.6676 -0.0476 0.054 Uiso 1 1 calc R U . . .
C14 C 0.451(3) 0.929(3) 1.014(9) 0.074(18) Uani 1 1 d . U . . .
H14A H 0.4526 0.8960 1.1063 0.111 Uiso 1 1 calc R U . . .
H14B H 0.4272 0.9599 1.0725 0.111 Uiso 1 1 calc R U . . .
H14C H 0.4899 0.9432 0.9877 0.111 Uiso 1 1 calc R U . . .
C15 C 0.281(2) 0.769(2) -0.264(8) 0.053(12) Uani 1 1 d . U . . .
H15A H 0.2661 0.7301 -0.2304 0.080 Uiso 1 1 calc R U . . .
H15B H 0.3116 0.7652 -0.3638 0.080 Uiso 1 1 calc R U . . .
H15C H 0.2490 0.7924 -0.3178 0.080 Uiso 1 1 calc R U . . .
N1 N 0.5769(10) 0.7719(15) 0.187(3) 0.044(3) Uani 0.62(4) 1 d D U P A 1
N2 N 0.4949(16) 0.7635(16) 0.533(6) 0.040(3) Uani 1 1 d . U . . .
N3 N 0.4527(16) 0.7232(16) 0.190(6) 0.041(3) Uani 1 1 d . U . . .
O1 O 0.5613(18) 0.8213(17) 0.229(7) 0.044(3) Uani 0.62(4) 1 d D U P A 1
O2 O 0.6205(13) 0.7623(18) 0.089(4) 0.044(3) Uani 0.62(4) 1 d D U P A 1
O3 O 0.5680(16) 0.6094(19) 0.013(7) 0.081(13) Uani 1 1 d . U . . .
O4 O 0.6449(14) 0.6629(15) 0.576(5) 0.056(9) Uani 1 1 d . U . . .
O5 O 0.4693(18) 0.5954(18) 0.575(7) 0.082(14) Uani 1 1 d . U . . .
O6 O 0.4233(15) 0.9093(15) 0.825(6) 0.061(9) Uani 1 1 d . U . . .
O7 O 0.3043(14) 0.7968(15) -0.086(5) 0.048(8) Uani 1 1 d . U . . .
Re1 Re 0.53128(8) 0.69449(8) 0.3447(3) 0.0414(6) Uani 1 1 d D U . . .
O1A O 0.5618(14) 0.7744(10) 0.221(4) 0.044(3) Uani 0.38(4) 1 d D U P A 2
N1A N 0.6096(15) 0.784(2) 0.116(5) 0.044(3) Uani 0.38(4) 1 d D U P A 2
O2A O 0.631(2) 0.733(3) 0.062(7) 0.044(3) Uani 0.38(4) 1 d D U P A 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
C1 O3 1.20(6) . ?
C1 Re1 1.84(5) . ?
C2 O4 1.21(5) . ?
C2 Re1 1.86(5) . ?
C3 O5 1.19(6) . ?
C3 Re1 1.86(5) . ?
C4 N2 1.31(6) . ?
C4 C5 1.38(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(6) . ?
C5 H5 0.9300 . ?
C6 O6 1.38(6) . ?
C6 C7 1.40(7) . ?
C7 C8 1.39(6) . ?
C7 H7 0.9300 . ?
C8 N2 1.36(5) . ?
C8 C9 1.49(6) . ?
C9 N3 1.37(6) . ?
C9 C10 1.40(6) . ?
C10 C11 1.34(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.36(6) . ?
C11 O7 1.41(5) . ?
C12 C13 1.35(6) . ?
C12 H12 0.9300 . ?
C13 N3 1.40(7) . ?
C13 H13 0.9300 . ?
C14 O6 1.47(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.44(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N1 O2 1.199(14) . ?
N1 O1 1.201(14) . ?
N1 Re1 2.28(3) . ?
N2 Re1 2.15(4) . ?
N3 Re1 2.15(4) . ?
Re1 O1A 2.096(15) . ?
O1A N1A 1.298(15) . ?
N1A O2A 1.300(15) . ?

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
O3 C1 Re1 173(4) . . ?
O4 C2 Re1 177(4) . . ?
O5 C3 Re1 174(4) . . ?
N2 C4 C5 129(5) . . ?
N2 C4 H4 115.3 . . ?
C5 C4 H4 115.3 . . ?
C6 C5 C4 113(5) . . ?
C6 C5 H5 123.3 . . ?
C4 C5 H5 123.3 . . ?
C5 C6 O6 125(5) . . ?
C5 C6 C7 122(5) . . ?
O6 C6 C7 113(4) . . ?
C8 C7 C6 117(4) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
N2 C8 C7 123(4) . . ?
N2 C8 C9 115(4) . . ?
C7 C8 C9 122(4) . . ?
N3 C9 C10 123(4) . . ?
N3 C9 C8 114(4) . . ?
C10 C9 C8 123(4) . . ?
C11 C10 C9 117(4) . . ?
C11 C10 H10 121.5 . . ?
C9 C10 H10 121.5 . . ?
C10 C11 C12 123(5) . . ?
C10 C11 O7 115(4) . . ?
C12 C11 O7 122(4) . . ?
C13 C12 C11 118(5) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C12 C13 N3 123(5) . . ?
C12 C13 H13 118.4 . . ?
N3 C13 H13 118.4 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 N1 O1 122(2) . . ?
O2 N1 Re1 119(3) . . ?
O1 N1 Re1 118(2) . . ?
C4 N2 C8 115(4) . . ?
C4 N2 Re1 127(3) . . ?
C8 N2 Re1 118(3) . . ?
C9 N3 C13 115(4) . . ?
C9 N3 Re1 118(3) . . ?
C13 N3 Re1 127(3) . . ?
C6 O6 C14 114(4) . . ?
C11 O7 C15 116(4) . . ?
C1 Re1 C3 92(2) . . ?
C1 Re1 C2 86(2) . . ?
C3 Re1 C2 91(2) . . ?
C1 Re1 O1A 99.8(17) . . ?
C3 Re1 O1A 166.3(18) . . ?
C2 Re1 O1A 96.0(16) . . ?
C1 Re1 N3 96.8(18) . . ?
C3 Re1 N3 92.6(18) . . ?
C2 Re1 N3 175.5(17) . . ?
O1A Re1 N3 79.9(13) . . ?
C1 Re1 N2 170.7(18) . . ?
C3 Re1 N2 92.7(18) . . ?
C2 Re1 N2 102.1(18) . . ?
O1A Re1 N2 74.4(14) . . ?
N3 Re1 N2 75.2(15) . . ?
C1 Re1 N1 91.4(16) . . ?
C3 Re1 N1 176.0(18) . . ?
C2 Re1 N1 90.7(15) . . ?
N3 Re1 N1 85.5(11) . . ?
N2 Re1 N1 83.3(12) . . ?
N1A O1A Re1 129(3) . . ?
O1A N1A O2A 107.8(16) . . ?

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
N2 C4 C5 C6 -1(8) . . . . ?
C4 C5 C6 O6 -176(5) . . . . ?
C4 C5 C6 C7 -2(7) . . . . ?
C5 C6 C7 C8 6(7) . . . . ?
O6 C6 C7 C8 -178(4) . . . . ?
C6 C7 C8 N2 -9(7) . . . . ?
C6 C7 C8 C9 -180(4) . . . . ?
N2 C8 C9 N3 3(6) . . . . ?
C7 C8 C9 N3 174(4) . . . . ?
N2 C8 C9 C10 180(4) . . . . ?
C7 C8 C9 C10 -9(7) . . . . ?
N3 C9 C10 C11 0(7) . . . . ?
C8 C9 C10 C11 -176(4) . . . . ?
C9 C10 C11 C12 -1(7) . . . . ?
C9 C10 C11 O7 -177(4) . . . . ?
C10 C11 C12 C13 1(8) . . . . ?
O7 C11 C12 C13 177(4) . . . . ?
C11 C12 C13 N3 -1(7) . . . . ?
C5 C4 N2 C8 -2(8) . . . . ?
C5 C4 N2 Re1 175(4) . . . . ?
C7 C8 N2 C4 7(7) . . . . ?
C9 C8 N2 C4 178(4) . . . . ?
C7 C8 N2 Re1 -170(3) . . . . ?
C9 C8 N2 Re1 1(5) . . . . ?
C10 C9 N3 C13 0(7) . . . . ?
C8 C9 N3 C13 177(4) . . . . ?
C10 C9 N3 Re1 178(3) . . . . ?
C8 C9 N3 Re1 -5(5) . . . . ?
C12 C13 N3 C9 1(7) . . . . ?
C12 C13 N3 Re1 -177(4) . . . . ?
C5 C6 O6 C14 -2(7) . . . . ?
C7 C6 O6 C14 -178(5) . . . . ?
C10 C11 O7 C15 -176(4) . . . . ?
C12 C11 O7 C15 8(6) . . . . ?
Re1 O1A N1A O2A 13(5) . . . . ?

_refine_diff_density_max         2.613
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.228


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_240K
_database_code_depnum_ccdc_archive 'CCDC 1842789'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_THETM01_PSS_240K            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data = no data above
0.9 A resolution.
;
_vrf_PLAT973_PSS_240K            
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 2.32 eA-3
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
_vrf_PLAT090_PSS_240K            
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.54 Note
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
leading to overall loss of unique reflection data.
;
_vrf_PLAT342_PSS_240K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.05444 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.3926(19)
_cell_length_b                   22.3926(19)
_cell_length_c                   6.6569(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3338.0(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    1195
_cell_measurement_theta_min      3.6310
_cell_measurement_theta_max      23.4920

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.019
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.0116
-1 1 1 0.1206
1 -1 -1 0.1391
-1 1 0 0.0116
0 -1 0 0.0096
0 1 0 0.0096
_exptl_absorpt_coefficient_mu    7.326
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6200
_diffrn_reflns_av_unetI/netI     0.1582
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.877
_diffrn_reflns_theta_max         23.217
_diffrn_reflns_theta_full        23.217
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2377
_reflns_number_gt                1799
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0508P)²+110.1451P] 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 433 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2377
_refine_ls_number_parameters     237
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.1896
_refine_ls_wR_factor_gt          0.1673
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6386(17) 0.5586(16) 0.862(7) 0.046(5) Uani 1 1 d . U . . .
C2 C 0.6758(17) 0.6031(18) 0.516(7) 0.044(5) Uani 1 1 d . U . . .
C3 C 0.6309(18) 0.4924(17) 0.521(7) 0.045(5) Uani 1 1 d . U . . .
C4 C 0.7828(17) 0.5217(17) 0.299(6) 0.045(9) Uani 1 1 d . U . . .
H4 H 0.7617 0.5539 0.2460 0.054 Uiso 1 1 calc R U . . .
C5 C 0.8300(15) 0.5017(15) 0.193(6) 0.038(8) Uani 1 1 d . U . . .
H5 H 0.8427 0.5208 0.0769 0.046 Uiso 1 1 calc R U . . .
C6 C 0.8591(17) 0.4515(17) 0.265(6) 0.040(8) Uani 1 1 d . U . . .
C7 C 0.8417(17) 0.4255(17) 0.440(6) 0.040(8) Uani 1 1 d . U . . .
H7 H 0.8615 0.3919 0.4878 0.048 Uiso 1 1 calc R U . . .
C8 C 0.7956(15) 0.4488(16) 0.542(6) 0.032(6) Uani 1 1 d . U . . .
C9 C 0.7715(16) 0.4251(16) 0.737(5) 0.031(6) Uani 1 1 d . U . . .
C10 C 0.7937(16) 0.3740(16) 0.823(7) 0.040(8) Uani 1 1 d . U . . .
H10 H 0.8239 0.3528 0.7592 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7713(17) 0.3541(16) 1.004(6) 0.040(8) Uani 1 1 d . U . . .
C12 C 0.7244(18) 0.3834(18) 1.082(6) 0.050(10) Uani 1 1 d . U . . .
H12 H 0.7078 0.3697 1.2016 0.060 Uiso 1 1 calc R U . . .
C13 C 0.7006(17) 0.4321(16) 0.993(7) 0.043(8) Uani 1 1 d . U . . .
H13 H 0.6684 0.4514 1.0524 0.051 Uiso 1 1 calc R U . . .
C14 C 0.926(2) 0.452(2) -0.015(7) 0.074(15) Uani 1 1 d . U . . .
H14A H 0.8922 0.4533 -0.1039 0.111 Uiso 1 1 calc R U . . .
H14B H 0.9567 0.4277 -0.0736 0.111 Uiso 1 1 calc R U . . .
H14C H 0.9407 0.4915 0.0071 0.111 Uiso 1 1 calc R U . . .
C15 C 0.7706(18) 0.2812(18) 1.255(6) 0.047(10) Uani 1 1 d . U . . .
H15A H 0.7322 0.2641 1.2259 0.071 Uiso 1 1 calc R U . . .
H15B H 0.7662 0.3126 1.3520 0.071 Uiso 1 1 calc R U . . .
H15C H 0.7965 0.2509 1.3078 0.071 Uiso 1 1 calc R U . . .
N1 N 0.7699(14) 0.5794(14) 0.809(5) 0.046(4) Uani 1 1 d . U . . .
N2 N 0.7637(13) 0.4986(13) 0.476(5) 0.039(4) Uani 1 1 d . U . . .
N3 N 0.7241(13) 0.4541(13) 0.810(5) 0.040(4) Uani 1 1 d . U . . .
O1 O 0.8225(13) 0.5629(15) 0.770(5) 0.079(11) Uani 1 1 d . U . . .
O2 O 0.7640(14) 0.6199(14) 0.926(5) 0.069(8) Uani 1 1 d . U . . .
O3 O 0.6072(17) 0.5687(15) 0.999(6) 0.093(12) Uani 1 1 d . U . . .
O4 O 0.6624(14) 0.6479(13) 0.429(5) 0.067(9) Uani 1 1 d . U . . .
O5 O 0.5939(16) 0.4690(16) 0.429(5) 0.091(12) Uani 1 1 d . U . . .
O6 O 0.9080(12) 0.4264(11) 0.173(5) 0.057(8) Uani 1 1 d . U . . .
O7 O 0.7960(12) 0.3051(12) 1.074(4) 0.049(7) Uani 1 1 d . U . . .
Re1 Re 0.69440(7) 0.53387(7) 0.6605(3) 0.0423(5) Uani 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 O3 1.17(5) . ?
C1 Re1 1.92(4) . ?
C2 O4 1.20(4) . ?
C2 Re1 1.87(4) . ?
C3 O5 1.15(5) . ?
C3 Re1 1.94(4) . ?
C4 C5 1.35(5) . ?
C4 N2 1.36(5) . ?
C5 C6 1.38(5) . ?
C6 C7 1.36(5) . ?
C6 O6 1.37(4) . ?
C7 C8 1.34(5) . ?
C8 N2 1.40(4) . ?
C8 C9 1.50(5) . ?
C9 N3 1.34(5) . ?
C9 C10 1.37(5) . ?
C10 C11 1.38(6) . ?
C11 O7 1.31(4) . ?
C11 C12 1.34(5) . ?
C12 C13 1.35(5) . ?
C13 N3 1.42(6) . ?
C14 O6 1.43(5) . ?
C15 O7 1.44(4) . ?
N1 O2 1.20(4) . ?
N1 O1 1.26(4) . ?
N1 Re1 2.21(3) . ?
N2 Re1 2.13(3) . ?
N3 Re1 2.15(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
O3 C1 Re1 172(4) . . ?
O4 C2 Re1 178(4) . . ?
O5 C3 Re1 177(4) . . ?
C5 C4 N2 125(4) . . ?
C4 C5 C6 118(4) . . ?
C7 C6 O6 116(3) . . ?
C7 C6 C5 121(4) . . ?
O6 C6 C5 124(4) . . ?
C8 C7 C6 119(4) . . ?
C7 C8 N2 123(4) . . ?
C7 C8 C9 125(3) . . ?
N2 C8 C9 112(3) . . ?
N3 C9 C10 123(3) . . ?
N3 C9 C8 115(3) . . ?
C10 C9 C8 122(3) . . ?
C9 C10 C11 120(4) . . ?
O7 C11 C12 127(4) . . ?
O7 C11 C10 115(3) . . ?
C12 C11 C10 118(4) . . ?
C11 C12 C13 122(4) . . ?
C12 C13 N3 121(4) . . ?
O2 N1 O1 117(4) . . ?
O2 N1 Re1 124(3) . . ?
O1 N1 Re1 119(3) . . ?
C4 N2 C8 115(3) . . ?
C4 N2 Re1 126(2) . . ?
C8 N2 Re1 119(2) . . ?
C9 N3 C13 116(3) . . ?
C9 N3 Re1 119(3) . . ?
C13 N3 Re1 125(3) . . ?
C6 O6 C14 117(3) . . ?
C11 O7 C15 116(3) . . ?
C2 Re1 C1 88.6(18) . . ?
C2 Re1 C3 89.2(16) . . ?
C1 Re1 C3 89.8(18) . . ?
C2 Re1 N2 99.9(15) . . ?
C1 Re1 N2 170.4(15) . . ?
C3 Re1 N2 94.6(15) . . ?
C2 Re1 N3 174.2(16) . . ?
C1 Re1 N3 96.8(15) . . ?
C3 Re1 N3 92.9(14) . . ?
N2 Re1 N3 74.5(12) . . ?
C2 Re1 N1 91.0(15) . . ?
C1 Re1 N1 93.0(15) . . ?
C3 Re1 N1 177.2(17) . . ?
N2 Re1 N1 82.7(13) . . ?
N3 Re1 N1 86.6(12) . . ?

_refine_diff_density_max         2.134
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.196


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_1min_405nm
_database_code_depnum_ccdc_archive 'CCDC 1842774'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.4161(5)
_cell_length_b                   22.4161(5)
_cell_length_c                   6.6101(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3321.4(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2359
_cell_measurement_theta_min      3.6290
_cell_measurement_theta_max      27.5000

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0105
-1 1 0 0.0135
1 -1 0 0.0135
1 1 0 0.0164
-1 1 1 0.1144
1 -1 -1 0.1144
_exptl_absorpt_coefficient_mu    7.362
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6060
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.874
_diffrn_reflns_theta_max         25.658
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_point_group_measured_fraction_full 0.932
_reflns_number_total             2918
_reflns_number_gt                2579
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_max     0.837
_reflns_Friedel_fraction_full    0.851

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0207P)²+14.7637P] 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 888 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2918
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.0881
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      0.998
_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
C1 C 0.3595(7) 0.5571(7) 0.862(3) 0.030(3) Uani 1 1 d . U . . .
C2 C 0.3248(7) 0.6033(7) 0.510(2) 0.027(3) Uani 1 1 d . U . . .
C3 C 0.3677(7) 0.4920(7) 0.514(3) 0.029(3) Uani 1 1 d . U . . .
C4 C 0.2179(7) 0.5189(7) 0.296(2) 0.025(3) Uani 1 1 d . U . . .
H4 H 0.2392 0.5522 0.2445 0.030 Uiso 1 1 calc R U . . .
C5 C 0.1694(6) 0.4988(7) 0.184(3) 0.028(3) Uani 1 1 d . U . . .
H5 H 0.1575 0.5178 0.0617 0.034 Uiso 1 1 calc R U . . .
C6 C 0.1397(7) 0.4494(7) 0.260(2) 0.028(3) Uani 1 1 d . U . . .
C7 C 0.1580(6) 0.4232(7) 0.440(2) 0.023(3) Uani 1 1 d . U . . .
H7 H 0.1374 0.3898 0.4949 0.027 Uiso 1 1 calc R U . . .
C8 C 0.2069(6) 0.4468(7) 0.538(2) 0.022(3) Uani 1 1 d . U . . .
C9 C 0.2286(7) 0.4218(7) 0.732(2) 0.022(3) Uani 1 1 d . U . . .
C10 C 0.2056(6) 0.3736(6) 0.825(2) 0.025(3) Uani 1 1 d . U . . .
H10 H 0.1724 0.3534 0.7671 0.030 Uiso 1 1 calc R U . . .
C11 C 0.2304(6) 0.3529(6) 1.007(2) 0.019(3) Uani 1 1 d . U . . .
C12 C 0.2785(7) 0.3837(7) 1.085(2) 0.025(3) Uani 1 1 d . U . . .
H12 H 0.2970 0.3715 1.2077 0.030 Uiso 1 1 calc R U . . .
C13 C 0.2987(7) 0.4327(7) 0.981(2) 0.029(3) Uani 1 1 d . U . . .
H13 H 0.3321 0.4533 1.0350 0.035 Uiso 1 1 calc R U . . .
C14 C 0.0710(7) 0.4485(8) -0.016(2) 0.038(4) Uani 1 1 d . U . . .
H14A H 0.0611 0.4907 0.0023 0.058 Uiso 1 1 calc R U . . .
H14B H 0.0354 0.4267 -0.0605 0.058 Uiso 1 1 calc R U . . .
H14C H 0.1024 0.4446 -0.1183 0.058 Uiso 1 1 calc R U . . .
C15 C 0.2313(7) 0.2793(7) 1.267(2) 0.029(4) Uani 1 1 d . U . . .
H15A H 0.2352 0.3105 1.3702 0.043 Uiso 1 1 calc R U . . .
H15B H 0.2708 0.2634 1.2339 0.043 Uiso 1 1 calc R U . . .
H15C H 0.2060 0.2471 1.3190 0.043 Uiso 1 1 calc R U . . .
N2 N 0.2370(6) 0.4960(6) 0.4687(19) 0.026(2) Uani 1 1 d . U . . .
N3 N 0.2759(5) 0.4535(5) 0.814(2) 0.026(2) Uani 1 1 d . U . . .
O3 O 0.3923(6) 0.5689(6) 0.9914(19) 0.052(3) Uani 1 1 d . U . . .
O4 O 0.3372(5) 0.6464(5) 0.4232(17) 0.040(3) Uani 1 1 d . U . . .
O5 O 0.4058(6) 0.4697(5) 0.427(2) 0.053(4) Uani 1 1 d . U . . .
O6 O 0.0915(5) 0.4243(5) 0.1709(18) 0.038(3) Uani 1 1 d . U . . .
O7 O 0.2044(5) 0.3044(5) 1.0867(14) 0.028(2) Uani 1 1 d . U . . .
Re1 Re 0.30569(3) 0.53259(3) 0.65652(9) 0.02562(18) Uani 1 1 d . U . . .
N1 N 0.2274(7) 0.5803(9) 0.804(4) 0.0320(19) Uani 0.710(15) 1 d D U P A 1
O1 O 0.1773(6) 0.5629(6) 0.767(2) 0.0320(19) Uani 0.710(15) 1 d D U P A 1
O2 O 0.2368(7) 0.6210(8) 0.915(3) 0.0320(19) Uani 0.710(15) 1 d D U P A 1
N1A N 0.2199(14) 0.609(2) 0.911(8) 0.0320(19) Uani 0.290(15) 1 d D U P A 2
O1A O 0.2271(17) 0.5631(16) 0.795(7) 0.0320(19) Uani 0.290(15) 1 d D U P A 2
O2A O 0.2710(15) 0.6362(15) 0.924(5) 0.0320(19) Uani 0.290(15) 1 d D U P A 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
C1 O3 1.160(18) . ?
C1 Re1 1.896(17) . ?
C2 O4 1.157(17) . ?
C2 Re1 1.907(16) . ?
C3 O5 1.143(18) . ?
C3 Re1 1.911(16) . ?
C4 N2 1.321(18) . ?
C4 C5 1.39(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(2) . ?
C5 H5 0.9500 . ?
C6 O6 1.351(18) . ?
C6 C7 1.39(2) . ?
C7 C8 1.38(2) . ?
C7 H7 0.9500 . ?
C8 N2 1.371(18) . ?
C8 C9 1.477(19) . ?
C9 C10 1.35(2) . ?
C9 N3 1.386(19) . ?
C10 C11 1.40(2) . ?
C10 H10 0.9500 . ?
C11 O7 1.343(17) . ?
C11 C12 1.38(2) . ?
C12 C13 1.37(2) . ?
C12 H12 0.9500 . ?
C13 N3 1.30(2) . ?
C13 H13 0.9500 . ?
C14 O6 1.425(19) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.449(16) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.142(13) . ?
N3 Re1 2.160(12) . ?
Re1 O1A 2.10(4) . ?
Re1 N1 2.274(17) . ?
N1 O2 1.189(12) . ?
N1 O1 1.214(12) . ?
N1A O1A 1.297(14) . ?
N1A O2A 1.299(14) . ?

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
O3 C1 Re1 176.2(14) . . ?
O4 C2 Re1 178.9(15) . . ?
O5 C3 Re1 177.5(15) . . ?
N2 C4 C5 126.0(15) . . ?
N2 C4 H4 117.0 . . ?
C5 C4 H4 117.0 . . ?
C6 C5 C4 116.1(15) . . ?
C6 C5 H5 121.9 . . ?
C4 C5 H5 121.9 . . ?
O6 C6 C5 124.0(14) . . ?
O6 C6 C7 115.6(14) . . ?
C5 C6 C7 120.4(15) . . ?
C8 C7 C6 118.3(15) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
N2 C8 C7 122.8(14) . . ?
N2 C8 C9 115.8(13) . . ?
C7 C8 C9 121.4(14) . . ?
C10 C9 N3 121.8(13) . . ?
C10 C9 C8 125.0(14) . . ?
N3 C9 C8 113.2(13) . . ?
C9 C10 C11 120.3(14) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
O7 C11 C12 126.6(13) . . ?
O7 C11 C10 115.6(13) . . ?
C12 C11 C10 117.8(13) . . ?
C13 C12 C11 117.8(14) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
N3 C13 C12 125.6(15) . . ?
N3 C13 H13 117.2 . . ?
C12 C13 H13 117.2 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 116.4(13) . . ?
C4 N2 Re1 125.7(11) . . ?
C8 N2 Re1 117.8(10) . . ?
C13 N3 C9 116.6(14) . . ?
C13 N3 Re1 125.4(12) . . ?
C9 N3 Re1 118.0(10) . . ?
C6 O6 C14 118.4(12) . . ?
C11 O7 C15 117.2(12) . . ?
C1 Re1 C2 88.8(7) . . ?
C1 Re1 C3 91.6(7) . . ?
C2 Re1 C3 88.9(6) . . ?
C1 Re1 O1A 97.4(11) . . ?
C2 Re1 O1A 98.0(13) . . ?
C3 Re1 O1A 168.7(9) . . ?
C1 Re1 N2 169.4(6) . . ?
C2 Re1 N2 100.7(6) . . ?
C3 Re1 N2 93.1(6) . . ?
O1A Re1 N2 76.9(10) . . ?
C1 Re1 N3 95.2(6) . . ?
C2 Re1 N3 174.9(6) . . ?
C3 Re1 N3 94.1(6) . . ?
O1A Re1 N3 78.4(13) . . ?
N2 Re1 N3 75.0(5) . . ?
C1 Re1 N1 92.8(7) . . ?
C2 Re1 N1 90.0(8) . . ?
C3 Re1 N1 175.4(7) . . ?
N2 Re1 N1 82.7(5) . . ?
N3 Re1 N1 86.6(7) . . ?
O2 N1 O1 122.3(16) . . ?
O2 N1 Re1 119.2(12) . . ?
O1 N1 Re1 118.5(12) . . ?
O1A N1A O2A 107.4(15) . . ?
N1A O1A Re1 128(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 -1(2) . . . . ?
C4 C5 C6 O6 179.4(14) . . . . ?
C4 C5 C6 C7 1(2) . . . . ?
O6 C6 C7 C8 -180.0(14) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C6 C7 C8 N2 2(2) . . . . ?
C6 C7 C8 C9 179.4(13) . . . . ?
N2 C8 C9 C10 -179.6(15) . . . . ?
C7 C8 C9 C10 3(2) . . . . ?
N2 C8 C9 N3 1.2(18) . . . . ?
C7 C8 C9 N3 -176.3(14) . . . . ?
N3 C9 C10 C11 -2(2) . . . . ?
C8 C9 C10 C11 178.9(13) . . . . ?
C9 C10 C11 O7 -179.6(13) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
O7 C11 C12 C13 -179.8(14) . . . . ?
C10 C11 C12 C13 0(2) . . . . ?
C11 C12 C13 N3 1(3) . . . . ?
C5 C4 N2 C8 2(2) . . . . ?
C5 C4 N2 Re1 -173.3(11) . . . . ?
C7 C8 N2 C4 -2(2) . . . . ?
C9 C8 N2 C4 -179.8(12) . . . . ?
C7 C8 N2 Re1 173.3(11) . . . . ?
C9 C8 N2 Re1 -4.2(17) . . . . ?
C12 C13 N3 C9 -2(2) . . . . ?
C12 C13 N3 Re1 177.4(12) . . . . ?
C10 C9 N3 C13 3(2) . . . . ?
C8 C9 N3 C13 -177.8(13) . . . . ?
C10 C9 N3 Re1 -176.9(12) . . . . ?
C8 C9 N3 Re1 2.3(16) . . . . ?
C5 C6 O6 C14 2(2) . . . . ?
C7 C6 O6 C14 -179.0(14) . . . . ?
C12 C11 O7 C15 -4(2) . . . . ?
C10 C11 O7 C15 175.9(12) . . . . ?
O2A N1A O1A Re1 3(7) . . . . ?

_refine_diff_density_max         1.431
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.165


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_200K
_database_code_depnum_ccdc_archive 'CCDC 1842788'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT973_VT_200K             
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 1.57 eA-3
RESPONSE: Very weak high angle data and poor resolution and data quality as a
result of crystal irradiation with strong LED light for 4 h period 
(as discussed in main text). This reduced data quality likely leads to 
truncation errors and spurious peaks and holes close to the heavy metal.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.6358(9)
_cell_length_b                   22.6358(9)
_cell_length_c                   6.5964(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3379.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2336
_cell_measurement_theta_min      3.6030
_cell_measurement_theta_max      26.6350

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0105
-1 1 0 0.0135
1 -1 0 0.0135
-1 -1 0 0.0164
-1 1 -1 0.1144
1 -1 1 0.1144
_exptl_absorpt_coefficient_mu    7.235
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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.
;
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6019
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.846
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.957
_reflns_number_total             3044
_reflns_number_gt                2632
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_max     0.901
_reflns_Friedel_fraction_full    0.908

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0060P)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 936 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3044
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0559
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.945
_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
C1 C 0.6411(5) 0.5544(5) 0.857(2) 0.034(2) Uani 1 1 d . U . . .
C2 C 0.6763(6) 0.5999(6) 0.5068(19) 0.031(3) Uani 1 1 d . U . . .
C3 C 0.6319(6) 0.4915(6) 0.516(2) 0.033(3) Uani 1 1 d . U . . .
C4 C 0.7841(6) 0.5165(6) 0.2895(17) 0.034(3) Uani 1 1 d . U . . .
H4 H 0.7644 0.5502 0.2364 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8304(5) 0.4955(5) 0.185(2) 0.034(3) Uani 1 1 d . U . . .
H5 H 0.8420 0.5133 0.0605 0.041 Uiso 1 1 calc R U . . .
C6 C 0.8614(6) 0.4470(6) 0.260(2) 0.033(3) Uani 1 1 d . U . . .
C7 C 0.8416(6) 0.4223(6) 0.4371(19) 0.033(3) Uani 1 1 d . U . . .
H7 H 0.8609 0.3883 0.4894 0.040 Uiso 1 1 calc R U . . .
C8 C 0.7941(5) 0.4456(5) 0.5407(17) 0.025(2) Uani 1 1 d . U . . .
C9 C 0.7711(5) 0.4212(5) 0.7307(17) 0.024(2) Uani 1 1 d . U . . .
C10 C 0.7939(5) 0.3727(5) 0.8242(19) 0.029(3) Uani 1 1 d . U . . .
H10 H 0.8270 0.3530 0.7665 0.035 Uiso 1 1 calc R U . . .
C11 C 0.7695(6) 0.3518(5) 1.0028(17) 0.029(3) Uani 1 1 d . U . . .
C12 C 0.7206(5) 0.3808(5) 1.0810(18) 0.028(3) Uani 1 1 d . U . . .
H12 H 0.7021 0.3673 1.2016 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6994(6) 0.4297(5) 0.9801(18) 0.031(3) Uani 1 1 d . U . . .
H13 H 0.6660 0.4495 1.0351 0.037 Uiso 1 1 calc R U . . .
C14 C 0.9297(6) 0.4468(6) -0.0139(18) 0.045(4) Uani 1 1 d . U . . .
H14A H 0.8979 0.4469 -0.1147 0.067 Uiso 1 1 calc R U . . .
H14B H 0.9628 0.4231 -0.0641 0.067 Uiso 1 1 calc R U . . .
H14C H 0.9430 0.4874 0.0098 0.067 Uiso 1 1 calc R U . . .
C15 C 0.7690(6) 0.2802(6) 1.2717(19) 0.044(4) Uani 1 1 d . U . . .
H15A H 0.7289 0.2664 1.2413 0.066 Uiso 1 1 calc R U . . .
H15B H 0.7674 0.3106 1.3773 0.066 Uiso 1 1 calc R U . . .
H15C H 0.7930 0.2469 1.3193 0.066 Uiso 1 1 calc R U . . .
N2 N 0.7633(5) 0.4934(4) 0.4650(15) 0.0291(19) Uani 1 1 d . U . . .
N3 N 0.7232(4) 0.4511(4) 0.8089(16) 0.0277(19) Uani 1 1 d . U . . .
O3 O 0.6087(5) 0.5670(5) 0.9880(15) 0.060(3) Uani 1 1 d . U . . .
O4 O 0.6643(4) 0.6438(4) 0.4250(14) 0.047(3) Uani 1 1 d . U . . .
O5 O 0.5947(5) 0.4687(5) 0.4254(16) 0.065(3) Uani 1 1 d . U . . .
O6 O 0.9086(4) 0.4225(4) 0.1694(15) 0.048(2) Uani 1 1 d . U . . .
O7 O 0.7955(4) 0.3049(4) 1.0891(12) 0.038(2) Uani 1 1 d . U . . .
Re1 Re 0.69466(2) 0.52986(2) 0.65241(7) 0.02823(14) Uani 1 1 d . U . . .
N1 N 0.7737(8) 0.5762(11) 0.808(5) 0.0403(18) Uani 0.491(11) 1 d D U P A 1
O1 O 0.8230(7) 0.5615(8) 0.761(2) 0.0403(18) Uani 0.491(11) 1 d D U P A 1
O2 O 0.7644(8) 0.6183(10) 0.912(3) 0.0403(18) Uani 0.491(11) 1 d D U P A 1
N1A N 0.7828(8) 0.6068(10) 0.889(4) 0.0403(18) Uani 0.509(11) 1 d D U P A 2
O1A O 0.7717(8) 0.5603(8) 0.784(4) 0.0403(18) Uani 0.509(11) 1 d D U P A 2
O2A O 0.7349(7) 0.6374(7) 0.906(3) 0.0403(18) Uani 0.509(11) 1 d D U P A 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
C1 O3 1.172(15) . ?
C1 Re1 1.895(14) . ?
C2 O4 1.163(14) . ?
C2 Re1 1.900(13) . ?
C3 O5 1.154(15) . ?
C3 Re1 1.893(14) . ?
C4 C5 1.344(17) . ?
C4 N2 1.355(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(17) . ?
C5 H5 0.9500 . ?
C6 O6 1.347(15) . ?
C6 C7 1.369(16) . ?
C7 C8 1.377(17) . ?
C7 H7 0.9500 . ?
C8 N2 1.382(14) . ?
C8 C9 1.465(15) . ?
C9 C10 1.362(15) . ?
C9 N3 1.378(16) . ?
C10 C11 1.385(16) . ?
C10 H10 0.9500 . ?
C11 O7 1.341(14) . ?
C11 C12 1.386(17) . ?
C12 C13 1.378(16) . ?
C12 H12 0.9500 . ?
C13 N3 1.341(16) . ?
C13 H13 0.9500 . ?
C14 O6 1.412(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.457(13) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.150(10) . ?
N3 Re1 2.159(10) . ?
Re1 O1A 2.066(19) . ?
Re1 N1 2.31(2) . ?
N1 O2 1.196(12) . ?
N1 O1 1.205(13) . ?
N1A O1A 1.283(13) . ?
N1A O2A 1.291(13) . ?

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
O3 C1 Re1 176.6(12) . . ?
O4 C2 Re1 177.2(12) . . ?
O5 C3 Re1 177.5(13) . . ?
C5 C4 N2 125.0(13) . . ?
C5 C4 H4 117.5 . . ?
N2 C4 H4 117.5 . . ?
C4 C5 C6 119.2(12) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
O6 C6 C7 118.1(13) . . ?
O6 C6 C5 124.3(12) . . ?
C7 C6 C5 117.6(13) . . ?
C6 C7 C8 121.4(13) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 N2 121.0(11) . . ?
C7 C8 C9 123.9(12) . . ?
N2 C8 C9 115.1(11) . . ?
C10 C9 N3 121.6(11) . . ?
C10 C9 C8 123.8(12) . . ?
N3 C9 C8 114.6(11) . . ?
C9 C10 C11 120.6(12) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
O7 C11 C10 117.1(11) . . ?
O7 C11 C12 124.6(11) . . ?
C10 C11 C12 118.3(11) . . ?
C13 C12 C11 118.6(11) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N3 C13 C12 123.9(12) . . ?
N3 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 115.8(11) . . ?
C4 N2 Re1 126.4(9) . . ?
C8 N2 Re1 117.3(8) . . ?
C13 N3 C9 117.0(11) . . ?
C13 N3 Re1 125.5(9) . . ?
C9 N3 Re1 117.5(8) . . ?
C6 O6 C14 119.3(10) . . ?
C11 O7 C15 118.3(10) . . ?
C3 Re1 C1 89.7(6) . . ?
C3 Re1 C2 88.7(5) . . ?
C1 Re1 C2 88.6(5) . . ?
C3 Re1 O1A 170.5(6) . . ?
C1 Re1 O1A 98.2(7) . . ?
C2 Re1 O1A 96.8(8) . . ?
C3 Re1 N2 95.3(5) . . ?
C1 Re1 N2 169.5(5) . . ?
C2 Re1 N2 100.8(5) . . ?
O1A Re1 N2 76.1(6) . . ?
C3 Re1 N3 94.2(5) . . ?
C1 Re1 N3 95.4(5) . . ?
C2 Re1 N3 175.1(5) . . ?
O1A Re1 N3 79.7(7) . . ?
N2 Re1 N3 75.1(4) . . ?
C3 Re1 N1 177.6(8) . . ?
C1 Re1 N1 92.7(7) . . ?
C2 Re1 N1 90.8(10) . . ?
N2 Re1 N1 82.5(6) . . ?
N3 Re1 N1 86.1(9) . . ?
O2 N1 O1 121.9(17) . . ?
O2 N1 Re1 118.8(15) . . ?
O1 N1 Re1 118.6(15) . . ?
O1A N1A O2A 109.0(13) . . ?
N1A O1A Re1 131.6(12) . . ?

_refine_diff_density_max         1.009
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.137


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_210K
_database_code_depnum_ccdc_archive 'CCDC 1842787'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.5343(9)
_cell_length_b                   22.5343(9)
_cell_length_c                   6.6415(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3372.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    2326
_cell_measurement_theta_min      3.6150
_cell_measurement_theta_max      26.8000

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0105
-1 1 0 0.0135
1 -1 0 0.0135
-1 -1 0 0.0164
-1 1 -1 0.1144
1 -1 1 0.1144
_exptl_absorpt_coefficient_mu    7.251
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6021
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.858
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             3049
_reflns_number_gt                2628
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_max     0.903
_reflns_Friedel_fraction_full    0.909

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0116P)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 943 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3049
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0643
_refine_ls_wR_factor_gt          0.0600
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6398(6) 0.5564(6) 0.862(2) 0.037(3) Uani 1 1 d . U . . .
C2 C 0.6757(6) 0.6030(6) 0.511(2) 0.031(3) Uani 1 1 d . U . . .
C3 C 0.6330(6) 0.4922(6) 0.521(2) 0.035(3) Uani 1 1 d . U . . .
C4 C 0.7837(6) 0.5189(6) 0.2957(18) 0.033(3) Uani 1 1 d . U . . .
H4 H 0.7635 0.5516 0.2447 0.040 Uiso 1 1 calc R U . . .
C5 C 0.8312(5) 0.4980(5) 0.188(2) 0.031(3) Uani 1 1 d . U . . .
H5 H 0.8429 0.5159 0.0679 0.037 Uiso 1 1 calc R U . . .
C6 C 0.8609(6) 0.4498(6) 0.2625(19) 0.032(3) Uani 1 1 d . U . . .
C7 C 0.8413(6) 0.4238(6) 0.4382(19) 0.030(3) Uani 1 1 d . U . . .
H7 H 0.8604 0.3903 0.4877 0.037 Uiso 1 1 calc R U . . .
C8 C 0.7939(5) 0.4472(5) 0.5405(18) 0.025(2) Uani 1 1 d . U . . .
C9 C 0.7708(6) 0.4234(6) 0.7319(18) 0.026(3) Uani 1 1 d . U . . .
C10 C 0.7939(5) 0.3738(5) 0.8221(19) 0.025(2) Uani 1 1 d . U . . .
H10 H 0.8255 0.3539 0.7627 0.030 Uiso 1 1 calc R U . . .
C11 C 0.7700(6) 0.3530(5) 1.0036(18) 0.026(2) Uani 1 1 d . U . . .
C12 C 0.7216(6) 0.3822(5) 1.0843(18) 0.029(3) Uani 1 1 d . U . . .
H12 H 0.7040 0.3692 1.2030 0.035 Uiso 1 1 calc R U . . .
C13 C 0.7003(6) 0.4312(5) 0.9841(18) 0.027(3) Uani 1 1 d . U . . .
H13 H 0.6674 0.4505 1.0374 0.033 Uiso 1 1 calc R U . . .
C14 C 0.9286(6) 0.4494(7) -0.011(2) 0.046(4) Uani 1 1 d . U . . .
H14A H 0.8987 0.4452 -0.1125 0.069 Uiso 1 1 calc R U . . .
H14B H 0.9641 0.4294 -0.0529 0.069 Uiso 1 1 calc R U . . .
H14C H 0.9370 0.4907 0.0100 0.069 Uiso 1 1 calc R U . . .
C15 C 0.7692(7) 0.2799(6) 1.2643(19) 0.042(4) Uani 1 1 d . U . . .
H15A H 0.7285 0.2702 1.2374 0.063 Uiso 1 1 calc R U . . .
H15B H 0.7711 0.3086 1.3711 0.063 Uiso 1 1 calc R U . . .
H15C H 0.7903 0.2447 1.3035 0.063 Uiso 1 1 calc R U . . .
N2 N 0.7643(4) 0.4954(4) 0.4711(15) 0.0280(19) Uani 1 1 d . U . . .
N3 N 0.7244(4) 0.4533(4) 0.8118(17) 0.0283(19) Uani 1 1 d . U . . .
O3 O 0.6086(5) 0.5688(5) 0.9907(17) 0.067(3) Uani 1 1 d . U . . .
O4 O 0.6631(4) 0.6460(4) 0.4279(14) 0.046(3) Uani 1 1 d . U . . .
O5 O 0.5950(5) 0.4699(4) 0.4296(16) 0.062(3) Uani 1 1 d . U . . .
O6 O 0.9082(4) 0.4241(4) 0.1709(16) 0.049(2) Uani 1 1 d . U . . .
O7 O 0.7960(4) 0.3044(4) 1.0854(12) 0.038(2) Uani 1 1 d . U . . .
Re1 Re 0.69456(2) 0.53229(2) 0.65691(7) 0.02735(14) Uani 1 1 d . U . . .
N1 N 0.7729(7) 0.5787(8) 0.809(4) 0.0382(17) Uani 0.690(12) 1 d D U P A 1
O1 O 0.8226(5) 0.5630(6) 0.7666(18) 0.0382(17) Uani 0.690(12) 1 d D U P A 1
O2 O 0.7630(6) 0.6191(7) 0.919(2) 0.0382(17) Uani 0.690(12) 1 d D U P A 1
N1A N 0.7820(11) 0.6116(15) 0.887(6) 0.0382(17) Uani 0.310(12) 1 d D U P A 2
O1A O 0.7687(14) 0.5644(14) 0.786(7) 0.0382(17) Uani 0.310(12) 1 d D U P A 2
O2A O 0.7331(12) 0.6412(12) 0.916(4) 0.0382(17) Uani 0.310(12) 1 d D U P A 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
C1 O3 1.144(15) . ?
C1 Re1 1.915(14) . ?
C2 O4 1.153(14) . ?
C2 Re1 1.911(13) . ?
C3 O5 1.164(15) . ?
C3 Re1 1.886(14) . ?
C4 N2 1.353(15) . ?
C4 C5 1.372(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.368(17) . ?
C5 H5 0.9300 . ?
C6 O6 1.356(16) . ?
C6 C7 1.377(16) . ?
C7 C8 1.373(16) . ?
C7 H7 0.9300 . ?
C8 N2 1.354(14) . ?
C8 C9 1.475(16) . ?
C9 N3 1.352(16) . ?
C9 C10 1.370(15) . ?
C10 C11 1.401(17) . ?
C10 H10 0.9300 . ?
C11 O7 1.356(13) . ?
C11 C12 1.381(17) . ?
C12 C13 1.376(16) . ?
C12 H12 0.9300 . ?
C13 N3 1.361(17) . ?
C13 H13 0.9300 . ?
C14 O6 1.411(15) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 O7 1.442(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N2 Re1 2.165(10) . ?
N3 Re1 2.164(10) . ?
Re1 O1A 2.01(3) . ?
Re1 N1 2.287(15) . ?
N1 O2 1.188(11) . ?
N1 O1 1.206(12) . ?
N1A O1A 1.294(14) . ?
N1A O2A 1.301(14) . ?

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
O3 C1 Re1 176.4(12) . . ?
O4 C2 Re1 178.0(12) . . ?
O5 C3 Re1 176.3(12) . . ?
N2 C4 C5 124.5(12) . . ?
N2 C4 H4 117.7 . . ?
C5 C4 H4 117.7 . . ?
C6 C5 C4 117.7(12) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
O6 C6 C5 124.0(12) . . ?
O6 C6 C7 116.8(13) . . ?
C5 C6 C7 119.2(13) . . ?
C8 C7 C6 120.4(13) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
N2 C8 C7 121.5(11) . . ?
N2 C8 C9 114.3(11) . . ?
C7 C8 C9 124.2(12) . . ?
N3 C9 C10 121.9(11) . . ?
N3 C9 C8 115.4(11) . . ?
C10 C9 C8 122.7(12) . . ?
C9 C10 C11 120.2(11) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
O7 C11 C12 124.8(11) . . ?
O7 C11 C10 116.7(11) . . ?
C12 C11 C10 118.5(11) . . ?
C13 C12 C11 118.1(12) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
N3 C13 C12 124.1(12) . . ?
N3 C13 H13 118.0 . . ?
C12 C13 H13 118.0 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 116.7(11) . . ?
C4 N2 Re1 125.1(9) . . ?
C8 N2 Re1 118.1(8) . . ?
C9 N3 C13 117.2(11) . . ?
C9 N3 Re1 117.7(8) . . ?
C13 N3 Re1 125.2(9) . . ?
C6 O6 C14 117.9(11) . . ?
C11 O7 C15 117.3(10) . . ?
C3 Re1 C2 89.6(5) . . ?
C3 Re1 C1 90.1(6) . . ?
C2 Re1 C1 88.8(6) . . ?
C3 Re1 O1A 170.8(8) . . ?
C2 Re1 O1A 95.8(12) . . ?
C1 Re1 O1A 97.5(10) . . ?
C3 Re1 N3 93.5(5) . . ?
C2 Re1 N3 174.6(5) . . ?
C1 Re1 N3 95.5(5) . . ?
O1A Re1 N3 80.6(12) . . ?
C3 Re1 N2 94.5(5) . . ?
C2 Re1 N2 101.2(5) . . ?
C1 Re1 N2 169.1(5) . . ?
O1A Re1 N2 77.2(9) . . ?
N3 Re1 N2 74.3(4) . . ?
C3 Re1 N1 176.8(6) . . ?
C2 Re1 N1 90.8(8) . . ?
C1 Re1 N1 93.1(6) . . ?
N3 Re1 N1 85.8(7) . . ?
N2 Re1 N1 82.3(5) . . ?
O2 N1 O1 122.8(15) . . ?
O2 N1 Re1 118.4(12) . . ?
O1 N1 Re1 118.7(11) . . ?
O1A N1A O2A 107.4(15) . . ?
N1A O1A Re1 135.2(18) . . ?

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
N2 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 O6 179.4(13) . . . . ?
C4 C5 C6 C7 1.5(19) . . . . ?
O6 C6 C7 C8 179.8(12) . . . . ?
C5 C6 C7 C8 -2.1(19) . . . . ?
C6 C7 C8 N2 1(2) . . . . ?
C6 C7 C8 C9 -178.4(12) . . . . ?
N2 C8 C9 N3 -1.0(16) . . . . ?
C7 C8 C9 N3 178.7(13) . . . . ?
N2 C8 C9 C10 178.1(12) . . . . ?
C7 C8 C9 C10 -2.3(19) . . . . ?
N3 C9 C10 C11 -0.7(19) . . . . ?
C8 C9 C10 C11 -179.7(11) . . . . ?
C9 C10 C11 O7 -178.7(11) . . . . ?
C9 C10 C11 C12 2.3(18) . . . . ?
O7 C11 C12 C13 179.7(11) . . . . ?
C10 C11 C12 C13 -1.4(18) . . . . ?
C11 C12 C13 N3 -1.0(19) . . . . ?
C5 C4 N2 C8 -1.1(19) . . . . ?
C5 C4 N2 Re1 174.3(10) . . . . ?
C7 C8 N2 C4 0.4(18) . . . . ?
C9 C8 N2 C4 -179.9(10) . . . . ?
C7 C8 N2 Re1 -175.4(10) . . . . ?
C9 C8 N2 Re1 4.3(14) . . . . ?
C10 C9 N3 C13 -1.6(18) . . . . ?
C8 C9 N3 C13 177.4(11) . . . . ?
C10 C9 N3 Re1 178.2(9) . . . . ?
C8 C9 N3 Re1 -2.8(14) . . . . ?
C12 C13 N3 C9 2.6(19) . . . . ?
C12 C13 N3 Re1 -177.2(9) . . . . ?
C5 C6 O6 C14 1(2) . . . . ?
C7 C6 O6 C14 179.2(12) . . . . ?
C12 C11 O7 C15 3.3(18) . . . . ?
C10 C11 O7 C15 -175.6(11) . . . . ?
O2A N1A O1A Re1 4(6) . . . . ?

_refine_diff_density_max         0.842
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.140


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_VT_175K
_database_code_depnum_ccdc_archive 'CCDC 1842786'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT973_VT_175K             
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 2.10 eA-3
RESPONSE: Very weak high angle data and poor resolution and data quality as a
result of crystal irradiation with strong LED light for 4 h period 
(as discussed in main text). This reduced data quality likely leads to 
truncation errors and spurious peaks and holes close to the heavy metal.
;
_vrf_PLAT342_VT_175K             
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03 Ang.
RESPONSE: Reduced data resolution and quality due to crystal irradiation for 
4 h period.
;
_vrf_PLAT972_VT_175K             
;
PROBLEM: Check Calcd Resid. Dens. 0.87A From Re1 -3.03 eA-3
RESPONSE: Very weak high angle data and poor resolution and data quality as a
result of crystal irradiation with strong LED light for 4 h period 
(as discussed in main text). This reduced data quality likely leads to 
truncation errors and spurious peaks and holes close to the heavy metal.
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.7219(11)
_cell_length_b                   22.7219(11)
_cell_length_c                   6.5890(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3401.8(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    1573
_cell_measurement_theta_min      3.6710
_cell_measurement_theta_max      25.9570

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.027
_exptl_crystal_size_min          0.027
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.0105
1 -1 0 0.0135
-1 1 0 0.0135
-1 -1 0 0.0164
1 -1 1 0.1144
-1 1 -1 0.1144
_exptl_absorpt_coefficient_mu    7.188
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            5838
_diffrn_reflns_av_unetI/netI     0.1297
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.835
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.952
_reflns_number_total             3036
_reflns_number_gt                2364
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_max     0.891
_reflns_Friedel_fraction_full    0.899

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)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 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3036
_refine_ls_number_parameters     235
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4463(9) 0.3598(9) 0.141(4) 0.038(3) Uani 1 1 d . U . . .
C2 C 0.4011(9) 0.3239(9) 0.496(3) 0.033(3) Uani 1 1 d . U . . .
C3 C 0.5083(10) 0.3680(10) 0.490(3) 0.038(4) Uani 1 1 d . U . . .
C4 C 0.4841(10) 0.2172(9) 0.711(3) 0.038(5) Uani 1 1 d . U . . .
H4 H 0.4500 0.2368 0.7597 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5061(8) 0.1696(9) 0.822(4) 0.035(4) Uani 1 1 d . U . . .
H5 H 0.4890 0.1579 0.9472 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5550(10) 0.1401(10) 0.738(3) 0.035(5) Uani 1 1 d . U . . .
C7 C 0.5798(9) 0.1580(9) 0.565(3) 0.034(4) Uani 1 1 d . U . . .
H7 H 0.6134 0.1383 0.5124 0.040 Uiso 1 1 calc R U . . .
C8 C 0.5555(9) 0.2063(9) 0.462(3) 0.035(5) Uani 1 1 d . U . . .
C9 C 0.5788(9) 0.2293(9) 0.272(3) 0.026(4) Uani 1 1 d . U . . .
C10 C 0.6280(8) 0.2058(8) 0.174(3) 0.029(4) Uani 1 1 d . U . . .
H10 H 0.6471 0.1720 0.2273 0.035 Uiso 1 1 calc R U . . .
C11 C 0.6482(9) 0.2310(9) 0.003(3) 0.030(4) Uani 1 1 d . U . . .
C12 C 0.6189(8) 0.2799(8) -0.085(3) 0.029(4) Uani 1 1 d . U . . .
H12 H 0.6316 0.2973 -0.2084 0.034 Uiso 1 1 calc R U . . .
C13 C 0.5702(9) 0.3008(9) 0.023(3) 0.032(4) Uani 1 1 d . U . . .
H13 H 0.5504 0.3344 -0.0299 0.039 Uiso 1 1 calc R U . . .
C14 C 0.5539(11) 0.0694(10) 1.015(3) 0.052(7) Uani 1 1 d . U . . .
H14A H 0.5123 0.0600 0.9952 0.078 Uiso 1 1 calc R U . . .
H14B H 0.5577 0.0996 1.1206 0.078 Uiso 1 1 calc R U . . .
H14C H 0.5752 0.0339 1.0571 0.078 Uiso 1 1 calc R U . . .
C15 C 0.7187(9) 0.2304(10) -0.274(3) 0.043(5) Uani 1 1 d . U . . .
H15A H 0.6871 0.2351 -0.3738 0.064 Uiso 1 1 calc R U . . .
H15B H 0.7494 0.2047 -0.3302 0.064 Uiso 1 1 calc R U . . .
H15C H 0.7357 0.2690 -0.2426 0.064 Uiso 1 1 calc R U . . .
N2 N 0.5082(7) 0.2362(7) 0.541(3) 0.033(2) Uani 1 1 d . U . . .
N3 N 0.5499(7) 0.2775(7) 0.190(3) 0.029(3) Uani 1 1 d . U . . .
O3 O 0.4339(7) 0.3917(8) 0.012(3) 0.064(5) Uani 1 1 d . U . . .
O4 O 0.3568(6) 0.3348(6) 0.579(2) 0.047(4) Uani 1 1 d . U . . .
O5 O 0.5312(7) 0.4060(7) 0.575(3) 0.057(5) Uani 1 1 d . U . . .
O6 O 0.5783(6) 0.0911(6) 0.829(2) 0.043(4) Uani 1 1 d . U . . .
O7 O 0.6953(6) 0.2044(6) -0.091(2) 0.040(4) Uani 1 1 d . U . . .
Re1 Re 0.47134(4) 0.30535(4) 0.35045(13) 0.0315(2) Uani 1 1 d . U . . .
N1 N 0.425(2) 0.2260(13) 0.197(9) 0.038(2) Uani 0.416(18) 1 d D U P A 1
O1 O 0.4394(14) 0.1771(13) 0.243(5) 0.038(2) Uani 0.416(18) 1 d D U P A 1
O2 O 0.3844(17) 0.2350(14) 0.083(6) 0.038(2) Uani 0.416(18) 1 d D U P A 1
N1A N 0.3941(12) 0.2167(9) 0.118(5) 0.038(2) Uani 0.584(18) 1 d D U P A 2
O1A O 0.4419(10) 0.2292(10) 0.215(5) 0.038(2) Uani 0.584(18) 1 d D U P A 2
O2A O 0.3637(9) 0.2644(10) 0.094(4) 0.038(2) Uani 0.584(18) 1 d D U P A 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
C1 O3 1.15(2) . ?
C1 Re1 1.94(2) . ?
C2 O4 1.17(2) . ?
C2 Re1 1.91(2) . ?
C3 O5 1.16(2) . ?
C3 Re1 1.89(2) . ?
C4 N2 1.32(2) . ?
C4 C5 1.40(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.41(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.34(3) . ?
C6 O6 1.37(2) . ?
C7 C8 1.40(3) . ?
C7 H7 0.9500 . ?
C8 N2 1.37(2) . ?
C8 C9 1.46(3) . ?
C9 N3 1.39(2) . ?
C9 C10 1.40(3) . ?
C10 C11 1.34(3) . ?
C10 H10 0.9500 . ?
C11 O7 1.38(2) . ?
C11 C12 1.42(3) . ?
C12 C13 1.40(3) . ?
C12 H12 0.9500 . ?
C13 N3 1.31(3) . ?
C13 H13 0.9500 . ?
C14 O6 1.43(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O7 1.45(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N2 Re1 2.178(17) . ?
N3 Re1 2.168(16) . ?
Re1 O1A 2.06(2) . ?
Re1 N1 2.32(4) . ?
N1 O1 1.199(10) . ?
N1 O2 1.20(4) . ?
N1A O1A 1.293(13) . ?
N1A O2A 1.295(13) . ?

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
O3 C1 Re1 176.8(19) . . ?
O4 C2 Re1 177.8(19) . . ?
O5 C3 Re1 179(2) . . ?
N2 C4 C5 123(2) . . ?
N2 C4 H4 118.3 . . ?
C5 C4 H4 118.3 . . ?
C4 C5 C6 116(2) . . ?
C4 C5 H5 121.8 . . ?
C6 C5 H5 121.8 . . ?
C7 C6 O6 117(2) . . ?
C7 C6 C5 121(2) . . ?
O6 C6 C5 121.4(19) . . ?
C6 C7 C8 119(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N2 C8 C7 120.9(19) . . ?
N2 C8 C9 115.6(18) . . ?
C7 C8 C9 124(2) . . ?
N3 C9 C10 119.9(18) . . ?
N3 C9 C8 116.6(18) . . ?
C10 C9 C8 123.5(19) . . ?
C11 C10 C9 119.9(19) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 O7 117.1(18) . . ?
C10 C11 C12 121.1(19) . . ?
O7 C11 C12 121.6(18) . . ?
C13 C12 C11 115.6(18) . . ?
C13 C12 H12 122.2 . . ?
C11 C12 H12 122.2 . . ?
N3 C13 C12 125(2) . . ?
N3 C13 H13 117.7 . . ?
C12 C13 H13 117.7 . . ?
O6 C14 H14A 109.5 . . ?
O6 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O6 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 N2 C8 118.9(19) . . ?
C4 N2 Re1 124.5(15) . . ?
C8 N2 Re1 116.1(13) . . ?
C13 N3 C9 118.8(18) . . ?
C13 N3 Re1 125.8(15) . . ?
C9 N3 Re1 115.4(13) . . ?
C6 O6 C14 120.1(17) . . ?
C11 O7 C15 118.9(16) . . ?
C3 Re1 C2 87.8(9) . . ?
C3 Re1 C1 89.7(10) . . ?
C2 Re1 C1 88.3(9) . . ?
C3 Re1 O1A 171.0(9) . . ?
C2 Re1 O1A 97.5(10) . . ?
C1 Re1 O1A 97.7(9) . . ?
C3 Re1 N3 95.2(8) . . ?
C2 Re1 N3 175.8(8) . . ?
C1 Re1 N3 94.6(8) . . ?
O1A Re1 N3 79.1(10) . . ?
C3 Re1 N2 95.3(8) . . ?
C2 Re1 N2 101.1(8) . . ?
C1 Re1 N2 169.5(8) . . ?
O1A Re1 N2 76.6(8) . . ?
N3 Re1 N2 75.8(6) . . ?
C3 Re1 N1 176.8(15) . . ?
C2 Re1 N1 90.5(16) . . ?
C1 Re1 N1 93.0(12) . . ?
N3 Re1 N1 86.3(14) . . ?
N2 Re1 N1 82.3(10) . . ?
O1 N1 O2 122(4) . . ?
O1 N1 Re1 119(3) . . ?
O2 N1 Re1 119(2) . . ?
O1A N1A O2A 109.0(14) . . ?
N1A O1A Re1 132.2(15) . . ?

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
N2 C4 C5 C6 -3(3) . . . . ?
C4 C5 C6 C7 2(3) . . . . ?
C4 C5 C6 O6 -177(2) . . . . ?
O6 C6 C7 C8 177(2) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C6 C7 C8 N2 2(3) . . . . ?
C6 C7 C8 C9 -180(2) . . . . ?
N2 C8 C9 N3 -2(3) . . . . ?
C7 C8 C9 N3 -180(2) . . . . ?
N2 C8 C9 C10 177.7(18) . . . . ?
C7 C8 C9 C10 0(3) . . . . ?
N3 C9 C10 C11 2(3) . . . . ?
C8 C9 C10 C11 -177.3(19) . . . . ?
C9 C10 C11 O7 -177.5(17) . . . . ?
C9 C10 C11 C12 -3(3) . . . . ?
C10 C11 C12 C13 3(3) . . . . ?
O7 C11 C12 C13 177.2(17) . . . . ?
C11 C12 C13 N3 -2(3) . . . . ?
C5 C4 N2 C8 4(3) . . . . ?
C5 C4 N2 Re1 174.8(15) . . . . ?
C7 C8 N2 C4 -3(3) . . . . ?
C9 C8 N2 C4 178.7(18) . . . . ?
C7 C8 N2 Re1 -175.1(16) . . . . ?
C9 C8 N2 Re1 7(2) . . . . ?
C12 C13 N3 C9 1(3) . . . . ?
C12 C13 N3 Re1 -176.0(14) . . . . ?
C10 C9 N3 C13 -1(3) . . . . ?
C8 C9 N3 C13 178.1(18) . . . . ?
C10 C9 N3 Re1 176.3(13) . . . . ?
C8 C9 N3 Re1 -4(2) . . . . ?
C7 C6 O6 C14 180(2) . . . . ?
C5 C6 O6 C14 -1(3) . . . . ?
C10 C11 O7 C15 -179.5(18) . . . . ?
C12 C11 O7 C15 6(3) . . . . ?
O2A N1A O1A Re1 6(5) . . . . ?

_refine_diff_density_max         1.849
_refine_diff_density_min         -2.476
_refine_diff_density_rms         0.205


_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_PSS_230K
_database_code_depnum_ccdc_archive 'CCDC 1842784'
_audit_update_record             
;
2018-05-11 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_THETM01_PSS_230K            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data = no data above
0.9 A resolution.
;
_vrf_PLAT973_PSS_230K            
;
PROBLEM: Check Calcd Positive Resid. Density on Re1 2.81 eA-3
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Weak / lack of high angle data likely
leading to truncation errors and termination ripples in data, particularly
around the heavy atom.
;
_vrf_PLAT090_PSS_230K            
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 5.72 Note
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
leading to overall loss of unique reflection data.
;
_vrf_PLAT342_PSS_230K            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.06 Ang.
RESPONSE: Reduced data quality due to irradiation damage - data collected
under continuous LED illumination. Loss of high angle data (above ~0.9 A)
;
# end Validation Reply Form

_chemical_name_systematic        
;
Nitro-(4,4'-dimethoxy-2,2'-bipyridine)-rhenium(I)-tricarbonyl
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H12 N3 O7 Re'
_chemical_formula_sum            'C15 H12 N3 O7 Re'
_chemical_formula_weight         532.48

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -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.
;

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

_cell_length_a                   22.581(2)
_cell_length_b                   22.581(2)
_cell_length_c                   6.6650(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3398.3(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    230(2)
_cell_measurement_reflns_used    1046
_cell_measurement_theta_min      3.5930
_cell_measurement_theta_max      27.9210

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.022
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0110
1 1 0 0.0214
-1 -1 0 0.0116
-1 -2 2 0.1260
1 -1 -1 0.1515
-2 1 1 0.1131
1 -1 0 0.0110
_exptl_absorpt_coefficient_mu    7.196
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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   ?
_diffrn_ambient_temperature      230(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6266
_diffrn_reflns_av_unetI/netI     0.1911
_diffrn_reflns_av_R_equivalents  0.1444
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.853
_diffrn_reflns_theta_max         23.237
_diffrn_reflns_theta_full        23.237
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2430
_reflns_number_gt                1617
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.988

_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_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0875P)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 342 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2430
_refine_ls_number_parameters     235
_refine_ls_number_restraints     263
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.2233
_refine_ls_wR_factor_gt          0.1922
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6386(18) 0.5572(17) 0.846(7) 0.045(4) Uani 1 1 d . U . . .
C2 C 0.6745(19) 0.601(2) 0.521(7) 0.049(4) Uani 1 1 d . U . . .
C3 C 0.6322(19) 0.4921(19) 0.518(7) 0.048(5) Uani 1 1 d . U . . .
C4 C 0.7841(18) 0.5186(19) 0.301(6) 0.046(8) Uani 1 1 d . U . . .
H4 H 0.7631 0.5509 0.2513 0.056 Uiso 1 1 calc R U . . .
C5 C 0.8312(17) 0.5019(19) 0.182(8) 0.051(9) Uani 1 1 d . U . . .
H5 H 0.8427 0.5219 0.0667 0.061 Uiso 1 1 calc R U . . .
C6 C 0.8606(19) 0.450(2) 0.259(6) 0.046(9) Uani 1 1 d . U . . .
C7 C 0.842(2) 0.426(2) 0.429(7) 0.060(12) Uani 1 1 d . U . . .
H7 H 0.8636 0.3946 0.4808 0.073 Uiso 1 1 calc R U . . .
C8 C 0.7926(19) 0.4466(19) 0.539(7) 0.047(8) Uani 1 1 d . U . . .
C9 C 0.7711(18) 0.4207(18) 0.729(6) 0.042(8) Uani 1 1 d . U . . .
C10 C 0.7940(18) 0.3724(18) 0.817(7) 0.048(9) Uani 1 1 d . U . . .
H10 H 0.8245 0.3519 0.7539 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7713(19) 0.3514(19) 1.010(7) 0.047(9) Uani 1 1 d . U . . .
C12 C 0.7224(19) 0.3817(18) 1.086(7) 0.049(9) Uani 1 1 d . U . . .
H12 H 0.7039 0.3681 1.2013 0.058 Uiso 1 1 calc R U . . .
C13 C 0.7013(17) 0.4318(17) 0.991(6) 0.039(7) Uani 1 1 d . U . . .
H13 H 0.6708 0.4530 1.0519 0.047 Uiso 1 1 calc R U . . .
C14 C 0.931(2) 0.451(2) -0.016(8) 0.087(19) Uani 1 1 d . U . . .
H14A H 0.8988 0.4539 -0.1105 0.130 Uiso 1 1 calc R U . . .
H14B H 0.9616 0.4269 -0.0705 0.130 Uiso 1 1 calc R U . . .
H14C H 0.9459 0.4901 0.0107 0.130 Uiso 1 1 calc R U . . .
C15 C 0.771(2) 0.283(2) 1.261(7) 0.064(13) Uani 1 1 d . U . . .
H15A H 0.7373 0.2602 1.2257 0.097 Uiso 1 1 calc R U . . .
H15B H 0.7591 0.3162 1.3430 0.097 Uiso 1 1 calc R U . . .
H15C H 0.7988 0.2594 1.3342 0.097 Uiso 1 1 calc R U . . .
N2 N 0.7624(14) 0.4968(14) 0.476(5) 0.045(3) Uani 1 1 d . U . . .
N3 N 0.7239(15) 0.4523(14) 0.805(6) 0.045(4) Uani 1 1 d . U . . .
O3 O 0.6088(15) 0.5696(15) 0.989(5) 0.077(10) Uani 1 1 d . U . . .
O4 O 0.6611(15) 0.6458(14) 0.423(5) 0.070(10) Uani 1 1 d . U . . .
O5 O 0.5935(16) 0.4681(15) 0.432(5) 0.083(12) Uani 1 1 d . U . . .
O6 O 0.9090(13) 0.4248(13) 0.172(5) 0.059(8) Uani 1 1 d . U . . .
O7 O 0.7990(13) 0.3052(14) 1.082(5) 0.060(8) Uani 1 1 d . U . . .
Re1 Re 0.69450(8) 0.53271(8) 0.6585(3) 0.0461(6) Uani 1 1 d D U . . .
N1 N 0.772(2) 0.5798(6) 0.8088(17) 0.052(3) Uani 0.74(4) 1 d . U P A 1
O1 O 0.8215(16) 0.5624(11) 0.775(3) 0.052(3) Uani 0.74(4) 1 d . U P A 1
O2 O 0.7627(17) 0.6218(13) 0.921(4) 0.052(3) Uani 0.74(4) 1 d . U P A 1
N1A N 0.776(3) 0.6109(15) 0.895(4) 0.052(3) Uani 0.26(4) 1 d D U P A 2
O1A O 0.7744(12) 0.5663(13) 0.773(3) 0.052(3) Uani 0.26(4) 1 d D U P A 2
O2A O 0.722(3) 0.6281(19) 0.927(6) 0.052(3) Uani 0.26(4) 1 d D U P A 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
C1 O3 1.20(5) . ?
C1 Re1 1.86(4) . ?
C2 O4 1.24(5) . ?
C2 Re1 1.85(5) . ?
C3 O5 1.18(5) . ?
C3 Re1 1.92(4) . ?
C4 N2 1.36(5) . ?
C4 C5 1.38(6) . ?
C5 C6 1.44(6) . ?
C6 C7 1.32(6) . ?
C6 O6 1.36(5) . ?
C7 C8 1.42(6) . ?
C8 N2 1.39(5) . ?
C8 C9 1.48(6) . ?
C9 C10 1.34(5) . ?
C9 N3 1.38(5) . ?
C10 C11 1.47(6) . ?
C11 O7 1.31(5) . ?
C11 C12 1.39(6) . ?
C12 C13 1.38(5) . ?
C13 N3 1.42(6) . ?
C14 O6 1.47(5) . ?
C15 O7 1.43(5) . ?
N2 Re1 2.12(3) . ?
N3 Re1 2.17(3) . ?
Re1 O1A 2.099(15) . ?
Re1 N1 2.28(4) . ?
N1 O1 1.21(5) . ?
N1 O2 1.23(4) . ?
N1A O1A 1.299(15) . ?
N1A O2A 1.302(15) . ?

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
O3 C1 Re1 169(4) . . ?
O4 C2 Re1 178(4) . . ?
O5 C3 Re1 179(4) . . ?
N2 C4 C5 132(4) . . ?
C4 C5 C6 112(4) . . ?
C7 C6 O6 117(4) . . ?
C7 C6 C5 119(4) . . ?
O6 C6 C5 124(4) . . ?
C6 C7 C8 124(5) . . ?
N2 C8 C7 120(4) . . ?
N2 C8 C9 115(4) . . ?
C7 C8 C9 125(4) . . ?
C10 C9 N3 124(4) . . ?
C10 C9 C8 125(4) . . ?
N3 C9 C8 111(4) . . ?
C9 C10 C11 121(4) . . ?
O7 C11 C12 130(4) . . ?
O7 C11 C10 114(4) . . ?
C12 C11 C10 116(4) . . ?
C13 C12 C11 121(4) . . ?
C12 C13 N3 123(4) . . ?
C4 N2 C8 112(4) . . ?
C4 N2 Re1 128(3) . . ?
C8 N2 Re1 120(3) . . ?
C9 N3 C13 115(4) . . ?
C9 N3 Re1 120(3) . . ?
C13 N3 Re1 124(3) . . ?
C6 O6 C14 118(3) . . ?
C11 O7 C15 112(4) . . ?
C2 Re1 C1 85.3(19) . . ?
C2 Re1 C3 88.8(18) . . ?
C1 Re1 C3 88(2) . . ?
C2 Re1 O1A 95.0(14) . . ?
C1 Re1 O1A 103.5(16) . . ?
C3 Re1 O1A 167.8(18) . . ?
C2 Re1 N2 102.3(17) . . ?
C1 Re1 N2 172.1(16) . . ?
C3 Re1 N2 93.9(15) . . ?
O1A Re1 N2 74.0(14) . . ?
C2 Re1 N3 175.7(17) . . ?
C1 Re1 N3 98.9(15) . . ?
C3 Re1 N3 92.6(15) . . ?
O1A Re1 N3 82.9(11) . . ?
N2 Re1 N3 73.5(13) . . ?
C2 Re1 N1 90.9(14) . . ?
C1 Re1 N1 95.0(15) . . ?
C3 Re1 N1 176.5(16) . . ?
N2 Re1 N1 82.8(12) . . ?
N3 Re1 N1 87.5(10) . . ?
O1 N1 O2 121(4) . . ?
O1 N1 Re1 118.6(16) . . ?
O2 N1 Re1 120(4) . . ?
O1A N1A O2A 107.7(16) . . ?
N1A O1A Re1 122(2) . . ?

_refine_diff_density_max         2.743
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.221


_chemical_properties_physical    Light-sensitive,Photo-sensitive
