Catalytic transfer zincation using ammonium cations.
Łosiewicz, Justyna; Bisai, Milan Kumar; Nichol, Gary S.; Macgregor, Stuart A.; Ingleson, Michael J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16697–16703; doi:10.1039/d5dt01816a

data_1575453
_publ_section_title
;
 Catalytic transfer zincation using ammonium cations.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16697
_journal_page_last               16703
_journal_paper_doi               10.1039/d5dt01816a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H47 B11 Br6 N2 Zn'
_chemical_formula_sum            'C30 H47 B11 Br6 N2 Zn'
_chemical_formula_weight         1099.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-30
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-05-27 deposited with the CCDC.	2025-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                64.066(4)
_cell_angle_beta                 76.749(4)
_cell_angle_gamma                75.510(4)
_cell_formula_units_Z            4
_cell_length_a                   11.6147(14)
_cell_length_b                   19.821(2)
_cell_length_c                   21.632(3)
_cell_measurement_reflns_used    4911
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.276
_cell_measurement_theta_min      2.320
_cell_volume                     4294.8(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       APEX4
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            289795
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.478
_diffrn_reflns_theta_min         2.126
_diffrn_source                   ImuS-Mo
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.179
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_correction_T_min  0.528053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0997 before and 0.0466 after correction.
 
For component 2:
 wR2(int) was 0.1111 before and 0.0511 after correction.
 The Ratio of minimum to maximum transmission is 0.71.

Final HKLF 4 output contains 289795 reflections, Rint = 0.0563
 (105290 with I > 3sig(I), Rint = 0.0383)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_recrystallization_method
'The material was recrystallised from pentane by slow evaporation'
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.333
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         29987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0380P)^2^+14.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24719
_reflns_number_total             29987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01816a3.cif
_cod_data_source_block           mi23012
_cod_depositor_comments          'Adding full bibliography for 1575453.cif.'
_cod_database_code               1575453
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.206
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5663(5)
 0.4337(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C62(H62), C65(H65), C74(H74), C77(H77)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C53(H53),
 C58(H58), C59(H59), C60(H60), C70(H70), C71(H71), C72(H72)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C51(H51A,H51B,H51C), C55(H55A,
 H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C)
3.d Boron cage BH refined with riding coordinates:
 C30(H30), B7(H7), B8(H8A), B9(H9A), B10(H10A), B11(H11), C80(H80), B57(H57),
 B58(H58A), B59(H59A), B60(H60A), B61(H61)
;
_shelx_res_checksum              28887
_shelx_hkl_checksum              9213
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id JL-067
_olex2_submission_special_instructions 'No special instructions were received'