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_1573068
_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         'C30 H39 I N4 Zn, 1[C6H14]'
_chemical_formula_sum            'C36 H53 I N4 Zn'
_chemical_formula_weight         734.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-29
_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                 91.3760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.60930(10)
_cell_length_b                   29.1368(3)
_cell_length_c                   14.2475(2)
_cell_measurement_reflns_used    36188
_cell_measurement_temperature    149.98(16)
_cell_measurement_theta_max      76.2620
_cell_measurement_theta_min      4.2730
_cell_volume                     3572.92(7)
_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      149.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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     -2.00  31.00   1.00    2.00    --  -41.65  19.00   0.00   33
  2  \w     -1.00  28.00   1.00    2.00    --  -41.65  19.00 150.00   29
  3  \w     -5.00  28.00   1.00    2.00    --  -41.65  19.00 120.00   33
  4  \w     -4.00  30.00   1.00    2.00    --  -41.65  19.00-120.00   34
  5  \w     -4.00  35.00   1.00    2.00    --  -41.65  19.00 -90.00   39
  6  \w     -5.00  37.00   1.00    2.00    --  -41.65  19.00  30.00   42
  7  \w     27.00  59.00   1.00    2.00    --   41.65-125.00  90.00   32
  8  \w     40.00  66.00   1.00   10.00    --  111.00 -45.00 120.00   26
  9  \w     46.00  71.00   1.00   10.00    --  111.00 -45.00  30.00   25
 10  \w     45.00  70.00   1.00   10.00    --  111.00 -45.00   0.00   25
 11  \w     39.00  94.00   1.00   10.00    --  111.00-111.00-150.00   55
 12  \w     54.00  84.00   1.00   10.00    --  111.00 -61.00   0.00   30
 13  \w     40.00  68.00   1.00   10.00    --  111.00 -45.00  90.00   28
 14  \w     77.00 103.00   1.00   10.00    --  111.00-111.00   0.00   26
 15  \w     63.00 100.00   1.00   10.00    --  111.00 178.00-150.00   37
 16  \w     48.00  74.00   1.00   10.00    --  111.00 -61.00-180.00   26
 17  \w    107.00 178.00   1.00   10.00    --  111.00 111.00 120.00   71
 18  \w     83.00 169.00   1.00   10.00    --  111.00  61.00-150.00   86
 19  \w    116.00 142.00   1.00   10.00    --  111.00  77.00-120.00   26
 20  \w    109.00 161.00   1.00   10.00    --  111.00  77.00-180.00   52
 21  \w    110.00 136.00   1.00   10.00    --  111.00 178.00-150.00   26
 22  \w     45.00 178.00   1.00   10.00    --  111.00   0.00-180.00  133
 23  \w    -21.00  19.00   1.00    2.00    --  -41.65  37.00 -30.00   40
 24  \w     31.00  89.00   1.00    2.00    --   41.65-125.00-180.00   58
 25  \w     44.00  73.00   1.00    2.00    --   41.65 -99.00   0.00   29
 26  \w     27.00  63.00   1.00    2.00    --   41.65-125.00   0.00   36
 27  \w     34.00  72.00   1.00    2.00    --   41.65-125.00 -90.00   38
 28  \w     73.00 117.00   1.00   10.00    --  111.00 178.00 -30.00   44
 29  \w     80.00 109.00   1.00   10.00    --  111.00-111.00  60.00   29
 30  \w     59.00  85.00   1.00   10.00    --  111.00-111.00 -90.00   26
 31  \w     41.00  67.00   1.00   10.00    --  111.00 -45.00  60.00   26
 32  \w     62.00 109.00   1.00   10.00    --  111.00-111.00 -30.00   47
 33  \w    105.00 144.00   1.00   10.00    --  111.00 111.00 -90.00   39
 34  \w     42.00 108.00   1.00   10.00    --  111.00-111.00 -60.00   66
 35  \w     46.00  72.00   1.00   10.00    --  111.00 -45.00-120.00   26
 36  \w     67.00 109.00   1.00   10.00    --  111.00-111.00 150.00   42
 37  \w    145.00 171.00   1.00   10.00    --  111.00  77.00-120.00   26
 38  \w    103.00 129.00   1.00   10.00    --  111.00  77.00-120.00   26
 39  \w     60.00  86.00   1.00   10.00    --  111.00-111.00   0.00   26
 40  \w     78.00 109.00   1.00   10.00    --  111.00-111.00-120.00   31
 41  \w    110.00 172.00   1.00   10.00    --  111.00  77.00  60.00   62
 42  \w    147.00 175.00   1.00   10.00    --  111.00  77.00 150.00   28
 43  \w     58.00 108.00   1.00   10.00    --  111.00-111.00  30.00   50
 44  \w     62.00 109.00   1.00   10.00    --  111.00-111.00-180.00   47
 45  \w     43.00  71.00   1.00   10.00    --  111.00 -45.00 -90.00   28
 46  \w    119.00 145.00   1.00   10.00    --  111.00 178.00 -60.00   26
 47  \w     69.00 107.00   1.00   10.00    --  111.00 -94.00  60.00   38
 48  \w     31.00  57.00   1.00   10.00    --  111.00 -94.00  60.00   26
 49  \w      0.00  25.00   1.00    2.00    --   34.00  86.00-110.45   25
 50  \w   -106.00 -19.00   1.00    2.00    --  -41.65 -37.00  60.00   87
 51  \w   -113.00 -19.00   1.00    2.00    --  -41.65 -37.00 -60.00   94
 52  \w   -102.00 -20.00   1.00    2.00    --  -41.65 -37.00-180.00   82
 53  \w     13.00  38.00   1.00    2.00    --   46.00  82.00-130.50   25
 54  \w     13.00  38.00   1.00    2.00    --   46.00  82.00  65.65   25
 55  \w     14.00  39.00   1.00    2.00    --   46.00  80.00 129.65   25
 56  \w     15.00  42.00   1.00    2.00    --   46.00  76.00 -37.05   27
 57  \w     33.00  59.00   1.00    2.00    --   62.00  69.00 169.38   26
 58  \w     32.00  90.00   1.00    2.00    --   62.00  71.00 -79.01   58
 59  \w     32.00  58.00   1.00    2.00    --   62.00  71.00 -28.52   26
 60  \w    106.00 134.00   1.00    2.00    --   62.00  71.00 -28.52   28
 61  \w     37.00  63.00   1.00    2.00    --   66.00  69.00 113.15   26
 62  \w     36.00  66.00   1.00    2.00    --   66.00  71.00-160.52   30
 63  \w     44.00  70.00   1.00    2.00    --   66.00  69.00  61.23   26
 64  \w     37.00  85.00   1.00    2.00    --   66.00  69.00-115.46   48
 65  \w     41.00  67.00   1.00    2.00    --   70.00  70.00   1.87   26
 66  \w     40.00  77.00   1.00    2.00    --   70.00  71.00  28.02   37
 67  \w    117.00 142.00   1.00    2.00    --   70.00  71.00 178.19   25
 68  \w     40.00  71.00   1.00    2.00    --   70.00  71.00 178.19   31
 69  \w     40.00  72.00   1.00    2.00    --   70.00  71.00  82.65   32
 70  \w     40.00  67.00   1.00    2.00    --   70.00  70.00 132.01   27
 71  \w     40.00  66.00   1.00    2.00    --   70.00  71.00 -29.58   26
 72  \w     83.00 127.00   1.00   10.00    --  111.00  61.00  90.00   44
 73  \w    123.00 177.00   1.00   10.00    --  111.00  61.00 -30.00   54
 74  \w     83.00 116.00   1.00   10.00    --  111.00  61.00 -30.00   33
 75  \w     83.00 116.00   1.00   10.00    --  111.00  61.00-180.00   33
 76  \w     83.00 142.00   1.00   10.00    --  111.00  61.00 -90.00   59
 77  \w    126.00 152.00   1.00   10.00    --  111.00  61.00  60.00   26
 78  \w    153.00 178.00   1.00   10.00    --  111.00  61.00  90.00   25
 79  \w     83.00 124.00   1.00   10.00    --  111.00  61.00  60.00   41
 80  \w     83.00 127.00   1.00   10.00    --  111.00  61.00 150.00   44
 81  \w     83.00 132.00   1.00   10.00    --  111.00  61.00 120.00   49
 82  \w    137.00 163.00   1.00   10.00    --  111.00  61.00-120.00   26
 83  \w    119.00 145.00   1.00   10.00    --  111.00  45.00-120.00   26
 84  \w     87.00 113.00   1.00   10.00    --  111.00  45.00-120.00   26
 85  \w     83.00 120.00   1.00   10.00    --  111.00  61.00-120.00   37
 86  \w     83.00 175.00   1.00   10.00    --  111.00  61.00  30.00   92
 87  \w     83.00 125.00   1.00   10.00    --  111.00  65.00 106.00   42
 88  \w    141.00 172.00   1.00   10.00    --  111.00  61.00 -60.00   31
 89  \w     83.00 125.00   1.00   10.00    --  111.00  61.00 -60.00   42
 90  \w     83.00 176.00   1.00   10.00    --  111.00  61.00   0.00   93
 91  \w     92.00 134.00   1.00   10.00    --  111.00  45.00   0.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303108000
_diffrn_orient_matrix_UB_12      -0.0305611000
_diffrn_orient_matrix_UB_13      0.0867960000
_diffrn_orient_matrix_UB_21      0.1295629000
_diffrn_orient_matrix_UB_22      -0.0252106000
_diffrn_orient_matrix_UB_23      -0.0520386000
_diffrn_orient_matrix_UB_31      0.1197336000
_diffrn_orient_matrix_UB_32      0.0350058000
_diffrn_orient_matrix_UB_33      0.0381931000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            79811
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.289
_diffrn_reflns_theta_min         4.341
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70358
_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    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0290P)^2^+1.5770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6790
_reflns_number_total             7460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06389a2.cif
_cod_data_source_block           089lglg24_auto
_cod_depositor_comments
'Adding full bibliography for 1573067--1573071.cif.'
_cod_database_code               1573068
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H50 Zn1'
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.504
_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:
 C28(H28), C25(H25), C27(H27), C24(H24), C3(H3), C10(H10), C8(H8), C19(H19),
 C17(H17)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C23(H23A,H23B,H23C), C1(H1A,H1B,
 H1C), C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C29(H29A,H29B,H29C), C21(H21A,H21B,
 H21C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 164 electrons were 
found in a volume of 844\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C6H14] per formula unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76249
_shelx_hkl_checksum              79273
_shelx_fab_checksum              35954
_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 1.484
_oxdiff_exptl_absorpt_empirical_full_min 0.799