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#$Date: 2023-05-04 08:23:17 +0300 (Thu, 04 May 2023) $
#$Revision: 282980 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712933.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7712933
loop_
_publ_author_name
'Stephens, Liam J.'
'Dallerba, Elena'
'Kelderman, Jenisi T. A.'
'Levina, Aviva'
'Werrett, Melissa V.'
'Lay, Peter A.'
'Massi, Massimiliano'
'Andrews, Philip C.'
_publ_section_title
;
 Synthesis and the photophysical and biological properties of tricarbonyl
 Re(I) diimine complexes bound to thiotetrazolato ligands.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4835
_journal_page_last               4848
_journal_paper_doi               10.1039/d2dt03237f
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         '2(C24 H18 N7 O3 Re S), C3 H6 O'
_chemical_formula_sum            'C51 H42 N14 O7 Re2 S2'
_chemical_formula_weight         1399.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                99.1100(10)
_cell_angle_beta                 91.2410(10)
_cell_angle_gamma                91.8400(10)
_cell_formula_units_Z            1
_cell_length_a                   6.79070(10)
_cell_length_b                   9.3555(2)
_cell_length_c                   19.8603(3)
_cell_measurement_reflns_used    13426
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.7420
_cell_measurement_theta_min      3.5920
_cell_volume                     1244.72(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23060
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.987
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       plate
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0185P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6137
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03237f2.cif
_cod_data_source_block           jk-1-11
_cod_database_code               7712933
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.466
_shelx_estimated_absorpt_t_max   0.906
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.98483(2) 0.61177(2) 0.66008(2) 0.01458(5) Uani 1 1 d . . . . .
S1 S 0.79233(13) 0.70085(9) 0.76564(5) 0.01852(18) Uani 1 1 d . . . . .
O1 O 0.7285(4) 0.7983(3) 0.58116(15) 0.0306(7) Uani 1 1 d . . . . .
O2 O 1.2996(4) 0.8587(3) 0.69371(16) 0.0307(6) Uani 1 1 d . U . . .
O3 O 1.2165(4) 0.5162(3) 0.53070(14) 0.0294(6) Uani 1 1 d . . . . .
O4 O 0.9352(11) 0.8714(10) 0.4306(4) 0.071(3) Uani 0.5 1 d . . P A -1
N3 N 0.8363(5) 0.4840(3) 0.84320(16) 0.0223(7) Uani 1 1 d . . . . .
N4 N 0.9566(5) 0.4583(3) 0.89539(17) 0.0250(7) Uani 1 1 d . . . . .
N5 N 1.0809(5) 0.5670(3) 0.91422(17) 0.0238(7) Uani 1 1 d . . . . .
N6 N 1.0411(4) 0.6662(3) 0.87311(16) 0.0199(6) Uani 1 1 d . . . . .
N7 N 1.4548(5) 1.1973(4) 0.94209(19) 0.0289(8) Uani 1 1 d . . . . .
N8 N 0.7796(4) 0.4237(3) 0.64538(15) 0.0155(6) Uani 1 1 d . . . . .
N9 N 1.1263(4) 0.4573(3) 0.71470(15) 0.0150(6) Uani 1 1 d . . . . .
C1 C 0.8879(5) 0.6131(4) 0.82894(18) 0.0171(7) Uani 1 1 d D U . . .
C2 C 1.1454(5) 0.8033(4) 0.88456(18) 0.0188(7) Uani 1 1 d . . . . .
C3 C 1.0475(5) 0.9258(4) 0.9103(2) 0.0232(8) Uani 1 1 d . . . . .
H6AA H 0.908790 0.919815 0.915358 0.028 Uiso 1 1 calc R U . . .
C4 C 1.1482(5) 1.0573(4) 0.9289(2) 0.0243(8) Uani 1 1 d . . . . .
H12 H 1.078396 1.140729 0.946780 0.029 Uiso 1 1 calc R U . . .
C5 C 1.3536(6) 1.0684(4) 0.9216(2) 0.0230(8) Uani 1 1 d . . . . .
C6 C 1.4484(5) 0.9427(4) 0.8913(2) 0.0238(8) Uani 1 1 d . . . . .
H0AA H 1.585158 0.948529 0.882586 0.029 Uiso 1 1 calc R U . . .
C7 C 1.3458(5) 0.8116(4) 0.8742(2) 0.0236(8) Uani 1 1 d . . . . .
H13 H 1.412696 0.727462 0.855428 0.028 Uiso 1 1 calc R U . . .
C8 C 1.3624(7) 1.3134(4) 0.9866(3) 0.0411(12) Uani 1 1 d . . . . .
H9A H 1.252944 1.349513 0.961913 0.062 Uiso 1 1 calc R U . . .
H9B H 1.459693 1.392501 1.001290 0.062 Uiso 1 1 calc R U . . .
H9C H 1.312346 1.276458 1.026735 0.062 Uiso 1 1 calc R U . . .
C9 C 1.6689(6) 1.2009(5) 0.9398(2) 0.0315(9) Uani 1 1 d . . . . .
H7AA H 1.721552 1.136611 0.969736 0.047 Uiso 1 1 calc R U . . .
H7AB H 1.720098 1.300081 0.955292 0.047 Uiso 1 1 calc R U . . .
H7AC H 1.709138 1.168491 0.892961 0.047 Uiso 1 1 calc R U . . .
C10 C 0.8268(5) 0.7307(4) 0.61131(19) 0.0205(7) Uani 1 1 d . . . . .
C11 C 1.1783(5) 0.7676(4) 0.68129(19) 0.0204(7) Uani 1 1 d . . . . .
C12 C 1.1260(5) 0.5484(4) 0.57937(19) 0.0183(7) Uani 1 1 d . . . . .
C13 C 0.6107(5) 0.4078(4) 0.60891(18) 0.0180(7) Uani 1 1 d . . . . .
H13A H 0.572036 0.483769 0.585494 0.022 Uiso 1 1 calc R U . . .
C14 C 0.4889(6) 0.2831(4) 0.6040(2) 0.0244(8) Uani 1 1 d . . . . .
H4AA H 0.371750 0.273750 0.576349 0.029 Uiso 1 1 calc R U . . .
C15 C 0.5396(5) 0.1740(4) 0.63945(19) 0.0218(8) Uani 1 1 d . . . . .
H14 H 0.455325 0.090389 0.637699 0.026 Uiso 1 1 calc R U . . .
C16 C 0.7156(5) 0.1868(4) 0.67802(18) 0.0185(7) Uani 1 1 d . . . . .
C17 C 0.8338(5) 0.3137(4) 0.67903(17) 0.0153(7) Uani 1 1 d . . . . .
C18 C 1.0178(5) 0.3307(4) 0.71524(18) 0.0158(7) Uani 1 1 d . . . . .
C19 C 1.0843(5) 0.2204(4) 0.74998(18) 0.0191(7) Uani 1 1 d . . . . .
C20 C 1.2687(6) 0.2431(4) 0.78429(19) 0.0244(8) Uani 1 1 d . . . . .
H0BA H 1.317749 0.171516 0.808627 0.029 Uiso 1 1 calc R U . . .
C21 C 1.3781(6) 0.3688(4) 0.78264(19) 0.0233(6) Uani 1 1 d D U . . .
H1BA H 1.504453 0.383849 0.804567 0.028 Uiso 1 1 calc R U . . .
C22 C 1.2997(5) 0.4740(4) 0.74809(18) 0.0196(7) Uani 1 1 d . . . . .
H4BA H 1.373958 0.561878 0.748459 0.023 Uiso 1 1 calc R U . . .
C23 C 0.7826(6) 0.0790(4) 0.71578(19) 0.0231(8) Uani 1 1 d . . . . .
H23 H 0.702986 -0.006086 0.716622 0.028 Uiso 1 1 calc R U . . .
C24 C 0.9584(6) 0.0963(4) 0.7505(2) 0.0233(6) Uani 1 1 d D U . . .
H24 H 0.998286 0.023568 0.775749 0.028 Uiso 1 1 calc R U . . .
C25 C 0.9808(13) 0.9621(10) 0.4781(5) 0.035(2) Uani 0.5 1 d . . P A -1
C26 C 1.148(3) 0.9515(15) 0.5221(13) 0.047(5) Uani 0.5 1 d . . P A -1
H21A H 1.184367 0.849948 0.518261 0.071 Uiso 0.5 1 calc R U P A -1
H21B H 1.115798 0.988079 0.569376 0.071 Uiso 0.5 1 calc R U P A -1
H21C H 1.259590 1.009144 0.508644 0.071 Uiso 0.5 1 calc R U P A -1
C27 C 0.857(4) 1.0976(16) 0.4918(12) 0.049(5) Uani 0.5 1 d . . P A -1
H24A H 0.788556 1.111753 0.449506 0.073 Uiso 0.5 1 calc R U P A -1
H24B H 0.943010 1.182442 0.508355 0.073 Uiso 0.5 1 calc R U P A -1
H24C H 0.759436 1.085067 0.526349 0.073 Uiso 0.5 1 calc R U P A -1
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Re1 C11 87.71(15) . . ?
C12 Re1 C10 90.24(15) . . ?
C11 Re1 C10 90.06(15) . . ?
C12 Re1 N9 92.11(12) . . ?
C11 Re1 N9 97.80(13) . . ?
C10 Re1 N9 171.87(13) . . ?
C12 Re1 N8 94.31(13) . . ?
C11 Re1 N8 173.52(13) . . ?
C10 Re1 N8 96.08(13) . . ?
N9 Re1 N8 75.99(10) . . ?
C12 Re1 S1 178.42(10) . . ?
C11 Re1 S1 92.12(11) . . ?
C10 Re1 S1 88.18(11) . . ?
N9 Re1 S1 89.47(8) . . ?
N8 Re1 S1 86.03(8) . . ?
C1 S1 Re1 105.36(12) . . ?
C1 N3 N4 107.4(3) . . ?
N5 N4 N3 110.9(3) . . ?
N4 N5 N6 106.0(3) . . ?
N5 N6 C1 108.9(3) . . ?
N5 N6 C2 119.3(3) . . ?
C1 N6 C2 131.6(3) . . ?
C5 N7 C9 118.8(3) . . ?
C5 N7 C8 119.9(3) . . ?
C9 N7 C8 117.9(3) . . ?
C13 N8 C17 118.4(3) . . ?
C13 N8 Re1 127.1(2) . . ?
C17 N8 Re1 114.4(2) . . ?
C22 N9 C18 118.1(3) . . ?
C22 N9 Re1 127.4(2) . . ?
C18 N9 Re1 114.5(2) . . ?
N3 C1 N6 106.8(3) . . ?
N3 C1 S1 128.3(3) . . ?
N6 C1 S1 124.9(3) . . ?
C3 C2 C7 120.2(3) . . ?
C3 C2 N6 119.5(3) . . ?
C7 C2 N6 120.2(3) . . ?
C2 C3 C4 120.9(3) . . ?
C3 C4 C5 120.4(3) . . ?
N7 C5 C4 120.6(3) . . ?
N7 C5 C6 122.0(3) . . ?
C4 C5 C6 117.4(3) . . ?
C7 C6 C5 121.2(3) . . ?
C6 C7 C2 119.7(3) . . ?
O1 C10 Re1 177.8(3) . . ?
O2 C11 Re1 177.9(3) . . ?
O3 C12 Re1 176.8(3) . . ?
N8 C13 C14 122.3(3) . . ?
C15 C14 C13 119.6(4) . . ?
C14 C15 C16 119.7(3) . . ?
C15 C16 C17 117.5(3) . . ?
C15 C16 C23 124.0(3) . . ?
C17 C16 C23 118.5(3) . . ?
N8 C17 C16 122.5(3) . . ?
N8 C17 C18 117.3(3) . . ?
C16 C17 C18 120.2(3) . . ?
N9 C18 C19 122.1(3) . . ?
N9 C18 C17 117.6(3) . . ?
C19 C18 C17 120.3(3) . . ?
C20 C19 C18 117.6(3) . . ?
C20 C19 C24 124.1(3) . . ?
C18 C19 C24 118.3(3) . . ?
C21 C20 C19 120.0(3) . . ?
C20 C21 C22 118.7(4) . . ?
N9 C22 C21 123.4(4) . . ?
C24 C23 C16 120.9(4) . . ?
C23 C24 C19 121.7(3) . . ?
O4 C25 C26 122.9(11) . . ?
O4 C25 C27 118.4(13) . . ?
C26 C25 C27 118.7(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C12 1.908(4) . ?
Re1 C11 1.920(4) . ?
Re1 C10 1.924(4) . ?
Re1 N9 2.174(3) . ?
Re1 N8 2.188(3) . ?
Re1 S1 2.5364(9) . ?
S1 C1 1.733(4) . ?
O1 C10 1.155(4) . ?
O2 C11 1.160(5) . ?
O3 C12 1.161(4) . ?
O4 C25 1.193(11) . ?
N3 C1 1.321(4) . ?
N3 N4 1.362(5) . ?
N4 N5 1.303(5) . ?
N5 N6 1.359(4) . ?
N6 C1 1.374(5) . ?
N6 C2 1.429(5) . ?
N7 C5 1.369(5) . ?
N7 C9 1.455(5) . ?
N7 C8 1.456(6) . ?
N8 C13 1.334(5) . ?
N8 C17 1.369(4) . ?
N9 C22 1.331(5) . ?
N9 C18 1.376(4) . ?
C2 C3 1.377(5) . ?
C2 C7 1.382(5) . ?
C3 C4 1.382(5) . ?
C4 C5 1.408(5) . ?
C5 C6 1.415(5) . ?
C6 C7 1.381(5) . ?
C13 C14 1.397(5) . ?
C14 C15 1.378(5) . ?
C15 C16 1.397(5) . ?
C16 C17 1.409(5) . ?
C16 C23 1.428(5) . ?
C17 C18 1.420(5) . ?
C18 C19 1.410(5) . ?
C19 C20 1.406(6) . ?
C19 C24 1.421(5) . ?
C20 C21 1.376(6) . ?
C21 C22 1.398(5) . ?
C23 C24 1.357(6) . ?
C25 C26 1.44(3) . ?
C25 C27 1.54(2) . ?
