A bis(silylene)pyridine pincer ligand can stabilize mononuclear manganese(0) complexes: facile access to isolable analogues of the elusive d7-Mn(CO)5 radical
Kalra, Shweta; Pividori, Daniel; Fehn, Dominik; Dai, Chenshu; Dong, Shicheng; Yao, Shenglai; Zhu, Jun; Meyer, Karsten; Driess, Matthias; Chemical Science 13 (2022) 8634–8641; doi:10.1039/D2SC03352F

data_1567399
_publ_section_title
;
 A bis(silylene)pyridine pincer ligand can stabilize mononuclear
 manganese(0) complexes: facile access to isolable analogues of the
 elusive d7-Mn(CO)5 radical
;
_journal_issue                   29
_journal_name_full               'Chemical Science'
_journal_page_first              8634
_journal_page_last               8641
_journal_paper_doi               10.1039/D2SC03352F
_journal_volume                  13
_journal_year                    2022
_chemical_formula_sum            'C48 H65 Mn N7 O3 Si2'
_chemical_formula_weight         899.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2c13q8
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-30 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.606(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1252(3)
_cell_length_b                   18.0882(5)
_cell_length_c                   13.3966(5)
_cell_measurement_reflns_used    3349
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.8790
_cell_measurement_theta_min      3.3690
_cell_volume                     2384.69(13)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Cu K\a'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9115
_diffrn_reflns_point_group_measured_fraction_full 0.702
_diffrn_reflns_point_group_measured_fraction_max 0.702
_diffrn_reflns_theta_full        67.485
_diffrn_reflns_theta_max         67.485
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'SuperNova, Single source at offset/far, Atlas'
_exptl_absorpt_coefficient_mu    3.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55718
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       'rectangular blocks'
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.019(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         6018
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+1.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.358
_reflns_Friedel_fraction_full    0.384
_reflns_Friedel_fraction_max     0.384
_reflns_number_gt                5332
_reflns_number_total             6018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03352f2.cif
_cod_data_source_block           CU-3991
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1567399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.499
_shelx_estimated_absorpt_t_max   0.688
_shelx_res_checksum              84938
_shelx_hkl_checksum              34836