Reductive C(sp3)–C(sp3) homo-coupling of benzyl or allyl halides with H2 using a water-soluble electron storage catalyst
Yatabe, Takeshi; Futakuchi, Sayaka; Miyazawa, Keishi; Shimauchi, Daiki; Takahashi, Yukina; Yoon, Ki-Seok; Nakai, Hidetaka; Ogo, Seiji; RSC Advances 11 (2021) 39450–39454; doi:10.1039/D1RA08596D

data_7244033
_publ_section_title
;
 Reductive C(sp3)--C(sp3) homo-coupling of benzyl or allyl halides with H2
 using a water-soluble electron storage catalyst
;
_journal_issue                   62
_journal_name_full               'RSC Advances'
_journal_page_first              39450
_journal_page_last               39454
_journal_paper_doi               10.1039/D1RA08596D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C24 H19 Cl N5 O2 Rh'
_chemical_formula_sum            'C24 H19 Cl N5 O2 Rh'
_chemical_formula_weight         547.80
_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     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-10-28 deposited with the CCDC.	2021-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                64.079(8)
_cell_angle_beta                 77.813(11)
_cell_angle_gamma                71.5960(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8230(10)
_cell_length_b                   11.1353(8)
_cell_length_c                   12.6467(12)
_cell_measurement_reflns_used    3575
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.20
_cell_volume                     1056.45(19)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b46'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b46'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34251
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         3.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.17
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4813
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3924
_reflns_number_total             4813
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1ra08596d2.cif
_cod_data_source_block           201027_RhL1Bz
_cod_database_code               7244033
_shelxl_version_number           2014/6
_shelx_res_checksum              81282