Zinc borylation and reduction by a diborane(4) species <i>via</i> B-O bond formation.
Griffin, Liam P.; Aldridge, Simon; Chemical science 15 (2024) 19577–19582; doi:10.1039/d4sc06389a

data_1573070
_publ_section_title
;
 Zinc borylation and reduction by a diborane(4) species <i>via</i> B-O
 bond formation.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              19577
_journal_page_last               19582
_journal_paper_doi               10.1039/d4sc06389a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C46 H58 N4 Zn2'
_chemical_formula_sum            'C46 H58 N4 Zn2'
_chemical_formula_weight         797.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-19 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7767(2)
_cell_length_b                   10.91670(10)
_cell_length_c                   36.1028(4)
_cell_measurement_reflns_used    37536
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3470
_cell_measurement_theta_min      2.4320
_cell_volume                     8582.71(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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     70.00 106.00   0.50   20.00    --   56.98  11.00  23.00   72
  2  \w     63.00  89.00   0.50   20.00    --   69.64 151.00   6.00   52
  3  \w     39.00  88.00   0.50   20.00    --   69.64-121.00  32.00   98
  4  \w     49.00  96.00   0.50   20.00    --   84.06  11.00  23.00   94
  5  \w     60.00 101.00   0.50   20.00    --   84.06-122.00 123.00   82
  6  \w     58.00  84.00   0.50   20.00    --   84.06-121.00  32.00   52
  7  \w     91.00 118.00   0.50   20.00    --   84.06 122.00-154.00   54
  8  \w     38.00  72.00   0.50   20.00    --   56.98 -94.00  60.00   68
  9  \w      4.00  29.00   0.50   20.00    --   56.98 -30.00 -90.00   50
 10  \w     54.00  98.00   0.50   20.00    --   56.98  30.00  60.00   88
 11  \w     12.00  37.00   0.50   20.00    --   56.98 -30.00-180.00   50
 12  \w     20.00  48.00   0.50   20.00    --   69.64 -45.00  60.00   56
 13  \w     25.00  50.00   0.50   20.00    --   69.64 -45.00  90.00   50
 14  \w     37.00  62.00   0.50   20.00    --   84.06 -61.00 120.00   50
 15  \w     46.00  71.00   0.50   20.00    --   84.06 -61.00  90.00   50
 16  \w     96.00 134.00   0.50   20.00    --   84.06  45.00-120.00   76
 17  \w     37.00  62.00   0.50   20.00    --   84.06 -61.00   0.00   50
 18  \w     69.00  99.00   0.50   20.00    --   84.06 -94.00 120.00   60
 19  \w     51.00  76.00   0.50   20.00    --   84.06 -94.00  30.00   50
 20  \w     68.00 105.00   0.50   20.00    --   84.06-111.00 120.00   74
 21  \w     43.00  69.00   0.50   20.00    --   84.06 -94.00   0.00   52
 22  \w     63.00  88.00   0.50   20.00    --   84.06 -94.00 -90.00   50
 23  \w     89.00 114.00   0.50   20.00    --   84.06  45.00 120.00   50
 24  \w     73.00  99.00   0.50   20.00    --   84.06 -94.00   0.00   52
 25  \w     43.00  68.00   0.50   20.00    --   84.06 -77.00-180.00   50
 26  \w     41.00  67.00   0.50   20.00    --   84.06-111.00-120.00   52
 27  \w     90.00 115.00   0.50   20.00    --   86.75  22.00 150.74   50
 28  \w     51.00  76.00   0.50   20.00    --   86.75  22.00 150.74   50
 29  \w     49.00 129.00   0.50   20.00    --   86.75   3.00-162.15  160
 30  \w     82.00 107.00   0.50   20.00    --   84.06 123.00-155.00   50
 31  \w     18.00  51.00   0.50   20.00    --   56.98-125.00-120.00   66
 32  \w     66.00  91.00   0.50   20.00    --   56.98-125.00-120.00   50
 33  \w      7.00  36.00   0.50   20.00    --   56.98 -30.00-150.00   58
 34  \w      4.00  29.00   0.50   20.00    --   56.98 -30.00  90.00   50
 35  \w     79.00 107.00   0.50   20.00    --   56.98  45.00 120.00   56
 36  \w     25.00  62.00   0.50   20.00    --   56.98 -94.00 120.00   74
 37  \w      7.00  33.00   0.50   20.00    --   56.98 -30.00   0.00   52
 38  \w     19.00  45.00   0.50   20.00    --   69.64 -45.00 120.00   52
 39  \w     49.00  75.00   0.50   20.00    --   69.64 -94.00 120.00   52
 40  \w     22.00  48.00   0.50   20.00    --   69.64 -45.00 -90.00   52
 41  \w     50.00  83.00   0.50   20.00    --   69.64 -94.00 -60.00   66
 42  \w     75.00 112.00   0.50   20.00    --   69.64  61.00  60.00   74
 43  \w     36.00  79.00   0.50   20.00    --   69.64 -94.00-150.00   86
 44  \w     19.00  44.00   0.50   20.00    --   69.64 -45.00-120.00   50
 45  \w     26.00  79.00   0.50   20.00    --   69.64 -94.00 -90.00  106
 46  \w     90.00 116.00   0.50   20.00    --   69.64  61.00 -60.00   52
 47  \w     20.00  46.00   0.50   20.00    --   69.64 -45.00 150.00   52
 48  \w     37.00  62.00   0.50   20.00    --   84.06 -61.00  30.00   50
 49  \w     47.00  74.00   0.50   20.00    --   84.06-111.00-180.00   54
 50  \w     69.00 108.00   0.50   20.00    --   84.06-111.00-120.00   78
 51  \w     43.00  68.00   0.50   20.00    --   84.06 -77.00-120.00   50
 52  \w     83.00 108.00   0.50   20.00    --   84.06-111.00 -60.00   50
 53  \w     43.00  68.00   0.50   20.00    --   84.06 -77.00  60.00   50
 54  \w     72.00  98.00   0.50   20.00    --   84.06 -94.00  90.00   52
 55  \w     52.00  99.00   0.50   20.00    --   84.06-111.00 -90.00   94
 56  \w     47.00  73.00   0.50   20.00    --   84.06 -77.00 -30.00   52
 57  \w     50.00  88.00   0.50   20.00    --   84.06 -77.00 -90.00   76
 58  \w     52.00  78.00   0.50   20.00    --   84.06 -77.00  30.00   52
 59  \w     95.00 121.00   0.50   20.00    --   84.06  45.00 150.00   52
 60  \w     78.00 108.00   0.50   20.00    --   84.06-111.00-180.00   60
 61  \w     43.00  68.00   0.50   20.00    --   84.06 -77.00   0.00   50
 62  \w    101.00 128.00   0.50   20.00    --   84.06 178.00  30.00   54
 63  \w     51.00  76.00   0.50   20.00    --   84.06 -94.00-150.00   50
 64  \w     55.00  81.00   0.50   20.00    --   84.06 -77.00-150.00   52
 65  \w     41.00  66.00   0.50   20.00    --   84.06 -61.00 -60.00   50
 66  \w     80.00 108.00   0.50   20.00    --   84.06-111.00  90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0196696000
_diffrn_orient_matrix_UB_12      0.0075517000
_diffrn_orient_matrix_UB_13      0.0409321000
_diffrn_orient_matrix_UB_21      -0.0675289000
_diffrn_orient_matrix_UB_22      -0.0182721000
_diffrn_orient_matrix_UB_23      -0.0114895000
_diffrn_orient_matrix_UB_31      0.0077678000
_diffrn_orient_matrix_UB_32      -0.1396687000
_diffrn_orient_matrix_UB_33      0.0037281000
_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  0.0747
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            130609
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.820
_diffrn_reflns_theta_min         2.448
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
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    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0803
_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^)+(0.0312P)^2^+46.4812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             8834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06389a2.cif
_cod_data_source_block           119lglg24_auto
_cod_depositor_comments
'Adding full bibliography for 1573067--1573071.cif.'
_cod_database_code               1573070
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 B1'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C40(H40), C17(H17), C3(H3), C19(H19), C8(H8), C31(H31), C26(H26),
 C33(H33), C10(H10)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C1(H1A,H1B,H1C), C46(H46A,H46B,H46C), C45(H45A,H45B,
 H45C), C28(H28A,H28B,H28C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C), C14(H14A,
 H14B,H14C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C35(H35A,H35B,H35C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C13(H13A,H13B,
 H13C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              98209
_shelx_hkl_checksum              61747
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.806
_oxdiff_exptl_absorpt_empirical_full_min 0.549