[(NHC)CoR<sub>2</sub>]: pre-catalysts for homogeneous olefin and alkyne hydrogenation.
Enachi, Andreea; Baabe, Dirk; Zaretzke, Marc-Kevin; Schweyen, Peter; Freytag, Matthias; Raeder, Jan; Walter, Marc D.; Chemical communications (Cambridge, England) 54 (2018) 13798–13801; doi:10.1039/c8cc08891h

data_7122652
_publ_section_title
;
 [(NHC)CoR<sub>2</sub>]: pre-catalysts for homogeneous olefin and alkyne
 hydrogenation.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13798
_journal_page_last               13801
_journal_paper_doi               10.1039/c8cc08891h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C31 H46 Co N2'
_chemical_formula_sum            'C31 H46 Co N2'
_chemical_formula_weight         505.63
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-25 deposited with the CCDC.
2018-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.88180(10)
_cell_length_b                   20.27730(10)
_cell_length_c                   11.91970(10)
_cell_measurement_reflns_used    42366
_cell_measurement_temperature    104(1)
_cell_measurement_theta_max      73.6250
_cell_measurement_theta_min      3.7200
_cell_volume                     2870.19(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -20.00  82.20   1.40    5.00    --   42.26 -99.00  30.00   73
  2  \w      2.00  97.20   1.40    5.00    --   42.26-125.00 -30.00   68
  3  \w    -30.00  69.40   1.40    5.00    --   42.26 -57.00 120.00   71
  4  \w     10.00 117.80   1.40    5.00    --   42.26  77.00-120.00   77
  5  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00  30.00   27
  6  \w     24.00 108.00   1.40   15.00    --  105.92 -94.00 150.00   60
  7  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00  60.00   27
  8  \w     24.00 108.00   1.40   15.00    --  105.92 -94.00 -60.00   60
  9  \w     33.00 119.80   1.40   15.00    --  105.92-125.00 -90.00   62
 10  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00 150.00   27
 11  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00 -60.00   27
 12  \w     24.00 108.00   1.40   15.00    --  105.92 -94.00  90.00   60
 13  \w     33.00  76.40   1.40   15.00    --  105.92 -45.00 -30.00   31
 14  \w     33.00  76.40   1.40   15.00    --  105.92 -45.00 -90.00   31
 15  \w     33.00  76.40   1.40   15.00    --  105.92 -45.00-150.00   31
 16  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00   0.00   27
 17  \w     33.00  76.40   1.40   15.00    --  105.92 -45.00  60.00   31
 18  \w     30.00 136.40   1.40   15.00    --  105.92 -77.00-180.00   76
 19  \w     33.00 119.80   1.40   15.00    --  105.92-125.00  90.00   62
 20  \w     24.00 158.40   1.40   15.00    --  105.92 -15.00-180.00   96
 21  \w     30.00  67.80   1.40   15.00    --  105.92 -30.00-180.00   27
 22  \w     80.00 178.00   1.40   15.00    --  105.92  45.00-180.00   70
 23  \w     24.00 108.00   1.40   15.00    --  105.92 -94.00   0.00   60
 24  \w   -118.00 -10.20   1.40    5.00    --  -42.26 -77.00 -60.00   77
 25  \w   -118.00 -10.20   1.40    5.00    --  -42.26 -77.00  30.00   77
 26  \w     14.00 114.80   1.40    5.00    --   42.26  57.00  90.00   72
 27  \w     14.00 114.80   1.40    5.00    --   42.26  57.00-180.00   72
 28  \w     14.00 114.80   1.40    5.00    --   42.26  57.00   0.00   72
 29  \w     80.00 178.00   1.40   15.00    --  105.92  45.00-120.00   70
 30  \w     73.00 178.00   1.40   15.00    --  105.92  77.00  60.00   75
 31  \w     78.00 177.40   1.40   15.00    --  105.92  30.00 -30.00   71
 32  \w     73.00 178.00   1.40   15.00    --  105.92  77.00 -30.00   75
 33  \w     73.00 178.00   1.40   15.00    --  105.92  77.00 -90.00   75
 34  \w     77.00 176.40   1.40   15.00    --  105.92  61.00 -90.00   71
 35  \w     73.00 178.00   1.40   15.00    --  105.92  77.00-180.00   75
 36  \w     73.00 178.00   1.40   15.00    --  105.92  77.00 -60.00   75
 37  \w     73.00 178.00   1.40   15.00    --  105.92  77.00  30.00   75
 38  \w     73.00 178.00   1.40   15.00    --  105.92  77.00  90.00   75
 39  \w     77.00 176.40   1.40   15.00    --  105.92  61.00 120.00   71
 40  \w     77.00 176.40   1.40   15.00    --  105.92  61.00 150.00   71
 41  \w     77.00 176.40   1.40   15.00    --  105.92  61.00-120.00   71
 42  \w     73.00 178.00   1.40   15.00    --  105.92  77.00   0.00   75
 43  \w     53.00 177.60   1.40   15.00    --  105.92  15.00  90.00   89
 44  \w   -118.00 -10.20   1.40    5.00    --  -42.26 -77.00  90.00   77
 45  \w   -118.00 -10.20   1.40    5.00    --  -42.26 -77.00-150.00   77
 46  \w   -118.00 -10.20   1.40    5.00    --  -42.26 -77.00 120.00   77
 47  \w   -117.00 -19.00   1.40    5.00    --  -42.26 -37.00  30.00   70
 48  \w     18.00 116.00   1.40    5.00    --   42.26  37.00   0.00   70
 49  \w     73.00 178.00   1.40   15.00    --  105.92  77.00-120.00   75
 50  \w     77.00 176.40   1.40   15.00    --  105.92  61.00-150.00   71
 51  \w     77.00 176.40   1.40   15.00    --  105.92  61.00-180.00   71
 52  \w     77.00 176.40   1.40   15.00    --  105.92  61.00 -30.00   71
 53  \w     80.00 178.00   1.40   15.00    --  105.92  45.00  90.00   70
 54  \w     77.00 176.40   1.40   15.00    --  105.92  61.00  90.00   71
 55  \w     77.00 176.40   1.40   15.00    --  105.92  61.00  30.00   71
 56  \w     77.00 176.40   1.40   15.00    --  105.92  61.00 -60.00   71
 57  \w     77.00 176.40   1.40   15.00    --  105.92  61.00   0.00   71
 58  \w     80.00 178.00   1.40   15.00    --  105.92  45.00 -90.00   70
 59  \w     73.00 178.00   1.40   15.00    --  105.92  77.00 120.00   75
 60  \w     73.00 178.00   1.40   15.00    --  105.92  77.00-150.00   75
 61  \w     80.00 178.00   1.40   15.00    --  105.92  45.00 -60.00   70
 62  \w     73.00 178.00   1.40   15.00    --  105.92  77.00 150.00   75
 63  \w     77.00 117.60   1.40   15.00    --  105.92  61.00  60.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143793000
_diffrn_orient_matrix_UB_12      -0.0503176000
_diffrn_orient_matrix_UB_13      -0.0953119000
_diffrn_orient_matrix_UB_21      -0.1094256000
_diffrn_orient_matrix_UB_22      -0.0346999000
_diffrn_orient_matrix_UB_23      0.0328260000
_diffrn_orient_matrix_UB_31      -0.0682058000
_diffrn_orient_matrix_UB_32      0.0451127000
_diffrn_orient_matrix_UB_33      -0.0810130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            102370
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.808
_diffrn_reflns_theta_min         3.722
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5806
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0420P)^2^+0.8067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5472
_reflns_number_total             5806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08891h2.cif
_cod_data_source_block           ae52ra
_cod_depositor_comments
'Adding full bibliography for 7122642--7122652.cif.'
_cod_database_code               7122652
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C31 H46 Co1 N2'
_chemical_oxdiff_usercomment     'hexane, -30degC'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C7 \\sim C4-C7A
 with sigma of 0.02
 C4-C6 \\sim C4-C6A
 with sigma of 0.02
 C4-C5 \\sim C4-C5A
 with sigma of 0.02
 C26-C31 \\sim C26-C31A
 with sigma of 0.02
 C26-C27A \\sim C26-C27
 with sigma of 0.02
 C31-C30 \\sim C31A-C30A
 with sigma of 0.02
 C27A-C28 \\sim C27-C28A
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C29-C28 \\sim C29A-C28A
 with sigma of 0.02
 C26-C30 \\sim C26-C30A
 with sigma of 0.04
 C26-C28 \\sim C26-C28A
 with sigma of 0.04
 C31-C29 \\sim C31A-C29A
 with sigma of 0.04
 C27A-C29 \\sim C27-C29A
 with sigma of 0.04
 C30-C28 \\sim C30A-C28A
 with sigma of 0.04
3. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=
 Sof(C31A)=Sof(H31A)=1-FVAR(2)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C27A)=Sof(H27A)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C27(H27),
 C28(H28), C29(H29), C30(H30), C31(H31), C27A(H27A), C28A(H28A), C29A(H29A),
 C30A(H30A), C31A(H31A)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,
 H6AC), C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              91785
_shelx_hkl_checksum              49004
_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 2.242
_oxdiff_exptl_absorpt_empirical_full_min 0.731