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_7713935
_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         'C20 H40 Na O8, C18 H26 B N2'
_chemical_formula_sum            'C38 H66 B N2 Na O8'
_chemical_formula_weight         712.72
_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             2023-05-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-04 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.047(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9715(4)
_cell_length_b                   12.8581(3)
_cell_length_c                   21.3987(5)
_cell_measurement_reflns_used    3469
_cell_measurement_temperature    100.03(13)
_cell_measurement_theta_max      73.2900
_cell_measurement_theta_min      3.0350
_cell_volume                     3978.12(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.943
_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    -19.00   6.00   1.00    2.00    --    5.00 -18.00 -25.00   25
  2  \w   -133.00-104.00   1.00    2.00    --  -45.40 -18.00 -25.00   29
  3  \w    -89.00  38.00   1.00    2.00    --  -45.40  18.00 143.00  127
  4  \w    -94.00 -25.00   1.00    4.00    -- -107.20  18.00 143.00   69
  5  \w   -197.00-105.00   1.00    4.00    -- -107.20 -18.00 -25.00   92
  6  \w    -68.00   8.00   1.00    2.00    --  -45.40  57.00-150.00   76
  7  \w   -133.00 -18.00   1.00    4.00    -- -107.20  76.00 -30.00  115
  8  \w   -147.00 -36.00   1.00    4.00    -- -107.20  38.00 -30.00  111
  9  \w   -122.00 -27.00   1.00    4.00    -- -107.20  57.00 -30.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035647000
_diffrn_orient_matrix_UB_12      0.0148437000
_diffrn_orient_matrix_UB_13      0.0720070000
_diffrn_orient_matrix_UB_21      -0.1041568000
_diffrn_orient_matrix_UB_22      0.0250169000
_diffrn_orient_matrix_UB_23      -0.0184012000
_diffrn_orient_matrix_UB_31      -0.0220131000
_diffrn_orient_matrix_UB_32      -0.1163193000
_diffrn_orient_matrix_UB_33      0.0052979000
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18533
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.000
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00045(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         7823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0439P)^2^+0.7860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5455
_reflns_number_total             7823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02896h2.cif
_cod_data_source_block           s5707r
_cod_original_cell_volume        3978.10(17)
_cod_database_code               7713935
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.889
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
;
_shelx_res_checksum              77000
_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 1.299
_oxdiff_exptl_absorpt_empirical_full_min 0.875