Efficient hydrogenation of ketones and aldehydes catalysed by a well-defined PNNP-rhenium complex.
Xu, Shuting; Zhang, Yu; Li, Bin; Li, Hao; Huang, Jing; Chen, Yiyu; Hu, Kun; Zhang, Fengjun; Fang, Xiaolong; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10396–10402; doi:10.1039/d5dt01368b

data_7718874
_publ_section_title
;
 Efficient hydrogenation of ketones and aldehydes catalysed by a
 well-defined PNNP-rhenium complex.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10396
_journal_page_last               10402
_journal_paper_doi               10.1039/d5dt01368b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C46 H44 N2 O2 P2 Re, Cl, 1.5[CH2Cl2]'
_chemical_formula_sum            'C47.5 H47 Cl4 N2 O2 P2 Re'
_chemical_formula_weight         1067.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-09 deposited with the CCDC.	2025-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0948(2)
_cell_length_b                   20.8238(5)
_cell_length_c                   32.3858(6)
_cell_measurement_reflns_used    25187
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.86
_cell_measurement_theta_min      3.98
_cell_volume                     8831.1(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      '452 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21094
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.745
_diffrn_reflns_theta_min         3.988
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.622
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.284
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1262P)^2^+13.3777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6911
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01368b2.cif
_cod_data_source_block           20231216-2
_cod_depositor_comments
'Adding full bibliography for 7718872--7718874.cif.'
_cod_original_formula_sum        'C47.50 H47 Cl4 N2 O2 P2 Re'
_cod_database_code               7718874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.479
_shelx_estimated_absorpt_t_min   0.358
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1), C00D(H00D), C013(H013)
2.b Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00B), C00P(H00C,H00E), C012(H01A,H01B), C014(H01C,H01D), C015(H01E,
 H01F), C016(H01G,H01H)
2.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00L(H00L), C00M(H00M), C00R(H00R), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C011(H011), C017(H017), C018(H018), C019(H019), C01A(H01I), C01B(H01J),
 C01C(H01K), C01D(H01L), C01E(H01M), C01F(H01N), C01G(H01O), C01H(H01P),
 C01I(H01Q), C01J(H01R), C01K(H01S), C01L(H01T)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22553
_shelx_hkl_checksum              26944
_shelx_fab_checksum              4707
_olex2_submission_special_instructions 'No special instructions were received'