Catalytic acceptorless dehydrogenation of alcohols using cobalt(i) pincer complexes supported by a P–GeH–P ligand
Liu, Yu-Chao; Cao, Dun-Xu; Ban, Qi-Yang; Ma, Wen-Jie; Xiao, Bin; Chemical Communications 61 (2025) 6917–6920; doi:10.1039/D5CC01050K

data_7134405
_publ_section_title
;
 Catalytic acceptorless dehydrogenation of alcohols using cobalt(i) pincer
 complexes supported by a P--GeH--P ligand
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_page_first              6917
_journal_page_last               6920
_journal_paper_doi               10.1039/D5CC01050K
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C36 H30 Ge P2'
_chemical_formula_sum            'C36 H30 Ge P2'
_chemical_formula_weight         597.13
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2mfxpp
_audit_creation_date             2022-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                95.058(2)
_cell_angle_beta                 113.143(3)
_cell_angle_gamma                108.781(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0280(4)
_cell_length_b                   12.8596(4)
_cell_length_c                   12.8744(3)
_cell_measurement_reflns_used    7688
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9920
_cell_measurement_theta_min      4.6460
_cell_volume                     1540.38(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2169
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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    -86.00 -57.00   1.00    1.00    --  -41.76 125.00 150.00   29
  2  \w    -70.00  29.00   1.00    1.00    --  -41.76  57.00  90.00   99
  3  \w   -112.00 -23.00   1.00    1.00    --  -41.76 -57.00 -60.00   89
  4  \w    -32.00  64.00   1.00    1.00    --   41.76 -38.00 150.00   96
  5  \w     49.00  75.00   1.00    1.00    --   41.76-125.00-180.00   26
  6  \w     39.00 108.00   1.00    3.00    --  106.05-125.00  30.00   69
  7  \w     77.00 129.00   1.00    3.00    --  106.05  61.00-150.00   52
  8  \w     30.00 115.00   1.00    3.00    --  106.05 -30.00-150.00   85
  9  \w     56.00 107.00   1.00    3.00    --  106.05 -94.00-120.00   51
 10  \w    104.00 166.00   1.00    3.00    --  106.05  77.00 150.00   62
 11  \w    114.00 175.00   1.00    3.00    --  106.05  77.00   0.00   61
 12  \w    116.00 143.00   1.00    3.00    --  106.05  77.00-150.00   27
 13  \w    142.00 167.00   1.00    3.00    --  106.05 125.00  60.00   25
 14  \w     86.00 112.00   1.00    3.00    --  106.05-125.00  60.00   26
 15  \w     74.00 107.00   1.00    3.00    --  106.05 -94.00  90.00   33
 16  \w     25.00 155.00   1.00    3.00    --  106.05 -15.00   0.00  130
 17  \w     42.00 135.00   1.00    3.00    --  106.05 -61.00   0.00   93
 18  \w     26.00 104.00   1.00    3.00    --  106.05 -94.00-180.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1229518000
_diffrn_orient_matrix_UB_12      -0.0302391000
_diffrn_orient_matrix_UB_13      -0.0032941000
_diffrn_orient_matrix_UB_21      0.1030259000
_diffrn_orient_matrix_UB_22      0.0810481000
_diffrn_orient_matrix_UB_23      0.1213621000
_diffrn_orient_matrix_UB_31      -0.0383685000
_diffrn_orient_matrix_UB_32      -0.0978017000
_diffrn_orient_matrix_UB_33      0.0573763000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10875
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.990
_diffrn_reflns_theta_min         3.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0069(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.2448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             5969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01050k2.cif
_cod_data_source_block           bqy-geh2_auto
_cod_depositor_comments
'Adding full bibliography for 7134401--7134405.cif.'
_cod_original_cell_volume        1540.37(9)
_cod_database_code               7134405
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         C20H20P1Ge1
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Rigid bond restraints
 C21, C22
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C24(H24), C10(H10), C5(H5), C30(H30), C36(H36), C2(H2), C26(H26),
 C3(H3), C8(H8), C4(H4), C9(H9), C28(H28), C14(H14), C18(H18), C20(H20),
 C32(H32), C29(H29), C23(H23), C27(H27), C22(H22), C35(H35), C15(H15), C17(H17),
  C21(H21), C33(H33), C16(H16), C34(H34)
;
_shelx_res_checksum              75143
_shelx_hkl_checksum              42228
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.778