Highly selective α-hydrogermylation of alkynes catalyzed by an in-situ generated bulky NHC–cobalt complex
Bołt, Małgorzata; Mermela, Aleksandra; Żak, Patrycja; Chemical Communications  (2023) –; doi:10.1039/D3CC03404F

data_7132083
_publ_section_title
;
 Highly selective \a-hydrogermylation of alkynes catalyzed by an in-situ
 generated bulky NHC--cobalt complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03404F
_journal_year                    2023
_chemical_formula_moiety         'C26 H21 F Ge'
_chemical_formula_sum            'C26 H21 F Ge'
_chemical_formula_weight         425.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-29 deposited with the CCDC.	2023-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.317(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1158(3)
_cell_length_b                   10.3844(3)
_cell_length_c                   19.5215(5)
_cell_measurement_reflns_used    5229
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.1280
_cell_measurement_theta_min      2.9380
_cell_volume                     2044.85(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.56a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     30.00  89.00   1.00   10.00    --   16.56  27.00  79.00   59
  2  \w    -52.00  49.00   1.00   10.00    --   16.56 -27.00 -83.00  101
  3  \w    -21.00   4.00   1.00   10.00    --  -17.42  27.00  79.00   25
  4  \w    -62.00 -37.00   1.00   10.00    --  -17.42 -27.00 -83.00   25
  5  \w     39.00  87.00   1.00   10.00    --   16.56 178.00 -90.00   48
  6  \w    -20.00  36.00   1.00   10.00    --   16.56 -99.00  90.00   56
  7  \w     -6.00  20.00   1.00   10.00    --   16.56  77.00   0.00   26
  8  \w    -13.00  31.00   1.00   10.00    --   16.56  77.00 150.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0653948000
_diffrn_orient_matrix_UB_12      -0.0244751000
_diffrn_orient_matrix_UB_13      0.0052363000
_diffrn_orient_matrix_UB_21      0.0058760000
_diffrn_orient_matrix_UB_22      0.0010710000
_diffrn_orient_matrix_UB_23      -0.0359780000
_diffrn_orient_matrix_UB_31      0.0251292000
_diffrn_orient_matrix_UB_32      0.0637564000
_diffrn_orient_matrix_UB_33      0.0026122000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         2.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.56a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0322P)^2^+1.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3449
_reflns_number_total             4435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03404f2.cif
_cod_data_source_block           gb1984_lt
_cod_original_cell_volume        2044.87(10)
_cod_database_code               7132083
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C16(H16), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              74985
_shelx_hkl_checksum              76185
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.186
_oxdiff_exptl_absorpt_empirical_full_min 0.930