A Robust Zintl Cluster for the Catalytic Reduction of Pyridines, Imines and Nitriles
van Ijzendoorn, Bono; Whittingham, Jessica; Whitehead, George F. S.; Kaltsoyannis, Nikolas; Mehta, Meera; Dalton Transactions  (2023) –; doi:10.1039/D3DT02896H

data_7713934
_publ_section_title
;
 A Robust Zintl Cluster for the Catalytic Reduction of Pyridines, Imines
 and Nitriles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02896H
_journal_year                    2023
_chemical_formula_moiety         'C18 H25 B N2'
_chemical_formula_sum            'C18 H25 B N2'
_chemical_formula_weight         280.21
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9457(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.52937(8)
_cell_length_b                   12.24923(11)
_cell_length_c                   13.53962(11)
_cell_measurement_reflns_used    13045
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.9600
_cell_measurement_theta_min      4.6230
_cell_volume                     1576.70(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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     46.00  84.00   1.00    1.00    --   46.08  28.00  72.00   38
  2  \w     88.00 169.00   1.00    1.00    --  108.20  28.00  72.00   81
  3  \w     40.00  65.00   1.00    1.00    --  108.20  28.00  72.00   25
  4  \w     19.00  44.00   1.00    1.00    --   43.52  28.00  72.00   25
  5  \w    -41.00  32.00   1.00    1.00    --   46.08  20.00-180.00   73
  6  \w    -40.00  69.00   1.00    1.00    --   46.08  40.00-150.00  109
  7  \w     85.00 111.00   1.00    1.00    --   46.08  40.00-150.00   26
  8  \w      9.00 134.00   1.00    1.00    --   46.08  20.00 -90.00  125
  9  \w    -42.00 131.00   1.00    1.00    --   46.08  60.00-120.00  173
 10  \w    -40.00 -15.00   1.00    1.00    --   46.08  60.00 150.00   25
 11  \w     22.00  48.00   1.00    1.00    --  108.20  50.00 120.00   26
 12  \w    152.00 179.00   1.00    1.00    --  108.20  40.00-150.00   27
 13  \w     19.00  45.00   1.00    1.00    --  108.20  50.00-180.00   26
 14  \w     20.00  45.00   1.00    1.00    --  108.20  40.00 120.00   25
 15  \w     20.00  45.00   1.00    1.00    --  108.20  30.00 150.00   25
 16  \w     20.00  45.00   1.00    1.00    --  108.20  50.00 150.00   25
 17  \w    130.00 188.00   1.00    1.00    --  108.20  50.00 150.00   58
 18  \w     99.00 125.00   1.00    1.00    --  108.20  40.00-150.00   26
 19  \w     19.00  46.00   1.00    1.00    --  108.20  40.00-150.00   27
 20  \w     68.00 197.00   1.00    1.00    --  108.20  20.00-120.00  129
 21  \w     21.00  55.00   1.00    1.00    --  108.20  41.00 165.86   34
 22  \w     19.00  45.00   1.00    1.00    --  108.20  56.00-159.94   26
 23  \w     20.00  47.00   1.00    1.00    --  108.20  40.00 150.00   27
 24  \w     19.00  91.00   1.00    1.00    --  108.20  42.00-128.35   72
 25  \w    108.00 198.00   1.00    1.00    --  108.20  42.00-128.35   90
 26  \w     75.00 198.00   1.00    1.00    --  108.20  40.00  90.00  123
 27  \w    173.00 198.00   1.00    1.00    --  108.20  50.00 120.00   25
 28  \w     19.00 162.00   1.00    1.00    --  108.20  50.00-120.00  143
 29  \w     20.00  87.00   1.00    1.00    --  108.20  40.00-180.00   67
 30  \w     20.00  45.00   1.00    1.00    --  108.20  50.00-150.00   25
 31  \w     25.00  81.00   1.00    1.00    --  108.20  30.00-150.00   56
 32  \w     19.00  88.00   1.00    1.00    --  108.20  30.00 120.00   69
 33  \w     51.00  76.00   1.00    1.00    --  108.20  20.00 150.00   25
 34  \w     82.00 109.00   1.00    1.00    --  108.20  50.00 120.00   27
 35  \w    111.00 136.00   1.00    1.00    --  108.20  50.00-180.00   25
 36  \w    172.00 198.00   1.00    1.00    --  108.20  28.00  72.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1418207000
_diffrn_orient_matrix_UB_12      -0.0561352000
_diffrn_orient_matrix_UB_13      -0.0282409000
_diffrn_orient_matrix_UB_21      -0.0446264000
_diffrn_orient_matrix_UB_22      0.0176384000
_diffrn_orient_matrix_UB_23      0.1060408000
_diffrn_orient_matrix_UB_31      -0.0646333000
_diffrn_orient_matrix_UB_32      0.1111230000
_diffrn_orient_matrix_UB_33      -0.0309979000
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19524
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.183
_diffrn_reflns_theta_min         4.651
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0521P)^2^+0.3850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3014
_reflns_number_total             3244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02896h2.cif
_cod_data_source_block           s5965l
_cod_database_code               7713934
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
;
_shelx_res_checksum              24278
_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 1.620
_oxdiff_exptl_absorpt_empirical_full_min 0.740