Synthesis and reactivity of N-heterocyclic carbene (NHC)-supported heavier nitrile ylides.
Sarkar, Debotra; Dutta, Sayan; Hanusch, Franziska; Koley, Debasis; Inoue, Shigeyoshi; Chemical science 15 (2024) 2391–2397; doi:10.1039/d3sc06430a

data_1570746
_publ_section_title
;
 Synthesis and reactivity of N-heterocyclic carbene (NHC)-supported
 heavier nitrile ylides.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2391
_journal_page_last               2397
_journal_paper_doi               10.1039/d3sc06430a
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C55 H63 N2 P Si Sn, 2(C4 H8 O)'
_chemical_formula_sum            'C63 H79 N2 O2 P Si Sn'
_chemical_formula_weight         1074.05
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_update_record
;
2023-10-10 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.462(10)
_cell_length_b                   15.316(11)
_cell_length_c                   14.954(9)
_cell_measurement_reflns_used    9508
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.2987
_cell_measurement_theta_min      2.4097
_cell_volume                     2831(3)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX III Control Software (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-201n (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS plate'
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Photon CMOS'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            93695
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.418
_exptl_crystal_size_min          0.267
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.027(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0204
_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^)+(0.0242P)^2^+0.9972P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                9807
_reflns_number_total             10314
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d3sc06430a2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 1570745--1570748.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1570746
_shelx_res_checksum              9463