Photocatalytic Deoxygenation of N‒O bonds with Rhenium Complexes: from the Reduction of Nitrous Oxide to Pyridine N-Oxides
Kjellberg, Marianne; Ohleier, Alexia; Thuéry, Pierre; Nicolas, Emmanuel; Anthore-Dalion, Lucile; Cantat, Thibault; Chemical Science  (2021) –; doi:10.1039/D1SC01974K

data_1563813
_publ_section_title
;
 Photocatalytic Deoxygenation of N--O bonds with Rhenium Complexes: from
 the Reduction of Nitrous Oxide to Pyridine N-Oxides
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01974K
_journal_year                    2021
_chemical_formula_sum            'C33 H32 Cl N2 O3.5 Re'
_chemical_formula_weight         734.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2021-01-14 deposited with the CCDC.	2021-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.166(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.2615(16)
_cell_length_b                   8.1575(3)
_cell_length_c                   22.7433(10)
_cell_measurement_reflns_used    155149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.58
_cell_volume                     5871.6(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 \f and 8 \w scans with 2\% steps (673 frames)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            155149
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_min         2.578
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.269
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+17.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4097
_reflns_number_total             5550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01974k2.cif
_cod_data_source_block           Re5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C33 H32 Cl N2 O3.50 Re'
_cod_database_code               1563813
_shelxl_version_number           2014-3
_shelx_res_checksum              15622
_shelx_hkl_checksum              61540