#------------------------------------------------------------------------------
#$Date: 2025-07-06 19:44:47 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300925 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/85/7718521.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_7718521
loop_
_publ_author_name
'Shee, Uday'
'Khutia, Biswajit'
'Ray, Sneha'
'Ghosh, Sumona'
'Rajak, Kajal Krishna'
_publ_section_title
;
 Highly efficient photocatalytic reduction of CO₂ to CO under
 visible light using rhenium benzo[d]oxazole complexes.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7294
_journal_page_last               7305
_journal_paper_doi               10.1039/d4dt03400g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C19 H10 Cl N2 O4 Re, 1[CH2Cl2]'
_chemical_formula_sum            'C20 H12 Cl3 N2 O4 Re'
_chemical_formula_weight         636.87
_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
_audit_creation_date             2024-07-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-19 deposited with the CCDC.	2025-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                96.3400(10)
_cell_angle_beta                 102.8560(10)
_cell_angle_gamma                110.7090(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4862(4)
_cell_length_b                   9.5540(4)
_cell_length_c                   13.1539(6)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.089
_cell_measurement_theta_min      2.330
_cell_volume                     1063.54(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26049
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.089
_diffrn_reflns_theta_max         25.089
_diffrn_reflns_theta_min         2.330
_exptl_absorpt_coefficient_mu    6.119
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1849 before and 0.0922 after correction.
The Ratio of minimum to maximum transmission is 0.6985.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3431
_reflns_number_total             3776
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt03400g3.cif
_cod_data_source_block           Complex-1c
_cod_depositor_comments
'Adding full bibliography for 7718520--7718524.cif.'
_cod_database_code               7718521
_shelx_shelxl_version_number     2016/6
_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_max   0.374
_shelx_estimated_absorpt_t_min   0.261
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C11(H11), C8(H8), C10(H10), C2(H2), C4(H4), C3(H3),
 C12(H12), C13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
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 0.54722(2) 0.49537(2) 0.26317(2) 0.03312(7) Uani 1 1 d . . . . .
Cl1 Cl 0.45048(15) 0.25437(14) 0.13071(10) 0.0557(3) Uani 1 1 d . . . . .
O1 O 0.9582(3) 0.4011(3) 0.3471(2) 0.0377(7) Uani 1 1 d . . . . .
N1 N 0.7352(4) 0.5716(4) 0.1842(3) 0.0352(8) Uani 1 1 d . . . . .
N2 N 0.7253(4) 0.4170(4) 0.3405(3) 0.0350(8) Uani 1 1 d . . . . .
O2 O 0.6758(4) 0.7952(4) 0.4240(3) 0.0605(10) Uani 1 1 d . . . . .
O4 O 0.3306(4) 0.6217(4) 0.1301(3) 0.0669(11) Uani 1 1 d . . . . .
O3 O 0.2987(4) 0.3721(4) 0.3799(3) 0.0757(12) Uani 1 1 d . . . . .
C19 C 0.6331(5) 0.6856(5) 0.3653(4) 0.0366(10) Uani 1 1 d . . . . .
C6 C 0.8458(4) 0.4501(5) 0.3034(3) 0.0342(10) Uani 1 1 d . . . . .
C7 C 0.9005(4) 0.3244(5) 0.4223(3) 0.0316(9) Uani 1 1 d . . . . .
C15 C 0.6707(5) 0.2650(5) 0.4847(3) 0.0371(10) Uani 1 1 d . . . . .
H15 H 0.574406 0.270387 0.483609 0.045 Uiso 1 1 calc R U . . .
C5 C 0.8615(5) 0.5344(5) 0.2189(3) 0.0358(10) Uani 1 1 d . . . . .
C14 C 0.7347(5) 0.1856(5) 0.5542(3) 0.0366(10) Uani 1 1 d . . . . .
C1 C 0.7374(5) 0.6480(5) 0.1057(4) 0.0431(11) Uani 1 1 d . . . . .
H1 H 0.651280 0.671946 0.079236 0.052 Uiso 1 1 calc R U . . .
C11 C 0.8593(6) 0.0234(5) 0.6877(4) 0.0535(13) Uani 1 1 d . . . . .
H11 H 0.899209 -0.031102 0.732198 0.064 Uiso 1 1 calc R U . . .
C16 C 0.7554(4) 0.3334(5) 0.4194(3) 0.0314(9) Uani 1 1 d . . . . .
C8 C 0.9669(5) 0.2493(5) 0.4853(3) 0.0379(10) Uani 1 1 d . . . . .
H8 H 1.062813 0.245022 0.483751 0.046 Uiso 1 1 calc R U . . .
C10 C 0.9401(5) 0.0933(5) 0.6235(4) 0.0468(12) Uani 1 1 d . . . . .
H10 H 1.035886 0.086832 0.624247 0.056 Uiso 1 1 calc R U . . .
C2 C 0.8596(5) 0.6930(5) 0.0617(4) 0.0484(12) Uani 1 1 d . . . . .
H2 H 0.856726 0.747754 0.007588 0.058 Uiso 1 1 calc R U . . .
C9 C 0.8822(5) 0.1772(5) 0.5540(3) 0.0369(10) Uani 1 1 d . . . . .
C17 C 0.4129(5) 0.5714(5) 0.1806(4) 0.0406(11) Uani 1 1 d . . . . .
C18 C 0.3938(5) 0.4177(5) 0.3361(4) 0.0465(12) Uani 1 1 d . . . . .
C4 C 0.9879(5) 0.5756(5) 0.1780(4) 0.0452(12) Uani 1 1 d . . . . .
H4 H 1.072415 0.548997 0.203900 0.054 Uiso 1 1 calc R U . . .
C3 C 0.9878(6) 0.6564(6) 0.0986(4) 0.0516(13) Uani 1 1 d . . . . .
H3 H 1.072300 0.686179 0.069791 0.062 Uiso 1 1 calc R U . . .
C12 C 0.7145(6) 0.0321(5) 0.6881(4) 0.0559(13) Uani 1 1 d . . . . .
H12 H 0.659742 -0.016365 0.733214 0.067 Uiso 1 1 calc R U . . .
C13 C 0.6530(6) 0.1109(5) 0.6230(4) 0.0504(12) Uani 1 1 d . . . . .
H13 H 0.556930 0.115298 0.624029 0.060 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Re1 Cl1 84.31(9) . . ?
N2 Re1 Cl1 84.54(9) . . ?
N2 Re1 N1 74.72(12) . . ?
C19 Re1 Cl1 177.06(11) . . ?
C19 Re1 N1 92.96(15) . . ?
C19 Re1 N2 93.72(15) . . ?
C17 Re1 Cl1 93.27(14) . . ?
C17 Re1 N1 96.04(15) . . ?
C17 Re1 N2 170.65(15) . . ?
C17 Re1 C19 88.08(18) . . ?
C17 Re1 C18 88.90(19) . . ?
C18 Re1 Cl1 93.92(15) . . ?
C18 Re1 N1 174.83(16) . . ?
C18 Re1 N2 100.30(16) . . ?
C18 Re1 C19 88.71(18) . . ?
C6 O1 C7 103.8(3) . . ?
C5 N1 Re1 116.4(3) . . ?
C1 N1 Re1 126.9(3) . . ?
C1 N1 C5 116.7(4) . . ?
C6 N2 Re1 114.3(3) . . ?
C6 N2 C16 104.3(3) . . ?
C16 N2 Re1 141.3(3) . . ?
O2 C19 Re1 176.7(4) . . ?
O1 C6 C5 120.8(4) . . ?
N2 C6 O1 116.7(4) . . ?
N2 C6 C5 122.5(4) . . ?
O1 C7 C16 107.9(3) . . ?
C8 C7 O1 127.2(4) . . ?
C8 C7 C16 124.9(4) . . ?
C14 C15 H15 121.1 . . ?
C16 C15 H15 121.1 . . ?
C16 C15 C14 117.8(4) . . ?
N1 C5 C6 112.0(4) . . ?
N1 C5 C4 122.8(4) . . ?
C4 C5 C6 125.1(4) . . ?
C15 C14 C9 120.4(4) . . ?
C13 C14 C15 120.8(4) . . ?
C13 C14 C9 118.8(4) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(4) . . ?
C2 C1 H1 118.3 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.3(5) . . ?
C12 C11 H11 119.9 . . ?
C7 C16 N2 107.3(3) . . ?
C15 C16 N2 132.3(4) . . ?
C15 C16 C7 120.3(4) . . ?
C7 C8 H8 121.9 . . ?
C7 C8 C9 116.2(4) . . ?
C9 C8 H8 121.9 . . ?
C11 C10 H10 119.3 . . ?
C11 C10 C9 121.3(4) . . ?
C9 C10 H10 119.3 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.3(4) . . ?
C3 C2 H2 120.4 . . ?
C8 C9 C14 120.5(4) . . ?
C8 C9 C10 121.2(4) . . ?
C10 C9 C14 118.4(4) . . ?
O4 C17 Re1 178.7(4) . . ?
O3 C18 Re1 178.7(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 H4 120.5 . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(4) . . ?
C4 C3 H3 120.6 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.0(5) . . ?
C13 C12 H12 119.5 . . ?
C14 C13 H13 119.9 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13 119.9 . . ?
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 Cl1 2.4673(12) . ?
Re1 N1 2.205(3) . ?
Re1 N2 2.179(3) . ?
Re1 C19 1.923(5) . ?
Re1 C17 1.882(5) . ?
Re1 C18 1.898(5) . ?
O1 C6 1.352(5) . ?
O1 C7 1.390(5) . ?
N1 C5 1.366(5) . ?
N1 C1 1.329(5) . ?
N2 C6 1.293(5) . ?
N2 C16 1.417(5) . ?
O2 C19 1.113(5) . ?
O4 C17 1.178(5) . ?
O3 C18 1.159(5) . ?
C6 C5 1.446(6) . ?
C7 C16 1.402(5) . ?
C7 C8 1.348(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.418(6) . ?
C15 C16 1.368(5) . ?
C5 C4 1.373(6) . ?
C14 C9 1.430(5) . ?
C14 C13 1.411(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.365(6) . ?
C11 H11 0.9300 . ?
C11 C10 1.341(6) . ?
C11 C12 1.407(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.417(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.424(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.382(6) . ?
C4 H4 0.9300 . ?
C4 C3 1.365(6) . ?
C3 H3 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.368(6) . ?
C13 H13 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 N1 C5 C6 -0.2(5) . . . . ?
Re1 N1 C5 C4 -179.3(3) . . . . ?
Re1 N1 C1 C2 179.1(3) . . . . ?
Re1 N2 C6 O1 -178.6(3) . . . . ?
Re1 N2 C6 C5 1.0(5) . . . . ?
Re1 N2 C16 C7 177.4(3) . . . . ?
Re1 N2 C16 C15 -1.2(8) . . . . ?
O1 C6 C5 N1 179.0(4) . . . . ?
O1 C6 C5 C4 -1.9(7) . . . . ?
O1 C7 C16 N2 0.2(4) . . . . ?
O1 C7 C16 C15 179.0(3) . . . . ?
O1 C7 C8 C9 -178.6(4) . . . . ?
N1 C5 C4 C3 -0.5(7) . . . . ?
N1 C1 C2 C3 1.1(8) . . . . ?
N2 C6 C5 N1 -0.6(6) . . . . ?
N2 C6 C5 C4 178.5(4) . . . . ?
C6 O1 C7 C16 -0.4(4) . . . . ?
C6 O1 C7 C8 177.5(4) . . . . ?
C6 N2 C16 C7 0.2(4) . . . . ?
C6 N2 C16 C15 -178.5(4) . . . . ?
C6 C5 C4 C3 -179.5(4) . . . . ?
C7 O1 C6 N2 0.6(5) . . . . ?
C7 O1 C6 C5 -179.0(4) . . . . ?
C7 C8 C9 C14 0.2(6) . . . . ?
C7 C8 C9 C10 179.4(4) . . . . ?
C15 C14 C9 C8 0.6(6) . . . . ?
C15 C14 C9 C10 -178.6(4) . . . . ?
C15 C14 C13 C12 178.7(5) . . . . ?
C5 N1 C1 C2 -1.9(7) . . . . ?
C5 C4 C3 C2 -0.4(8) . . . . ?
C14 C15 C16 N2 178.4(4) . . . . ?
C14 C15 C16 C7 -0.1(6) . . . . ?
C1 N1 C5 C6 -179.3(4) . . . . ?
C1 N1 C5 C4 1.6(6) . . . . ?
C1 C2 C3 C4 0.1(8) . . . . ?
C11 C10 C9 C14 0.0(7) . . . . ?
C11 C10 C9 C8 -179.2(4) . . . . ?
C11 C12 C13 C14 -0.2(8) . . . . ?
C16 N2 C6 O1 -0.5(5) . . . . ?
C16 N2 C6 C5 179.1(4) . . . . ?
C16 C7 C8 C9 -1.0(6) . . . . ?
C16 C15 C14 C9 -0.6(6) . . . . ?
C16 C15 C14 C13 -179.3(4) . . . . ?
C8 C7 C16 N2 -177.8(4) . . . . ?
C8 C7 C16 C15 1.0(7) . . . . ?
C10 C11 C12 C13 0.3(8) . . . . ?
C9 C14 C13 C12 0.0(7) . . . . ?
C12 C11 C10 C9 -0.2(7) . . . . ?
C13 C14 C9 C8 179.3(4) . . . . ?
C13 C14 C9 C10 0.1(6) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.582 0.000 0.000 251.1 87.4 '2 CH2Cl2'
