Contrasting reactivity of B-Cl and B-H bonds at [Ni(IMes)<sub>2</sub>] to form unsupported Ni-boryls.
Audsley, Gabrielle; Carpentier, Ambre; Pécharman, Anne-Frédérique; Wright, James; Roseveare, Thomas M.; Clark, Ewan R.; Macgregor, Stuart A.; Riddlestone, Ian M.; Chemical communications (Cambridge, England) 60 (2024) 874–877; doi:10.1039/d3cc05369e

data_7132488
_publ_section_title
;
 Contrasting reactivity of B-Cl and B-H bonds at [Ni(IMes)<sub>2</sub>] to
 form unsupported Ni-boryls.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              874
_journal_page_last               877
_journal_paper_doi               10.1039/d3cc05369e
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C52 H56 B Cl N6 Ni, C3.5 H4'
_chemical_formula_sum            'C55.5 H60 B Cl N6 Ni'
_chemical_formula_weight         916.06
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-04 deposited with the CCDC.	2023-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.570(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9362(6)
_cell_length_b                   11.3297(4)
_cell_length_c                   24.0854(9)
_cell_measurement_reflns_used    7570
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8900
_cell_measurement_theta_min      4.2120
_cell_volume                     4862.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2300
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.367
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         15659
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8929
_reflns_number_total             15659
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9982\% 
around [-0.08 -0.00 1.00] (reciprocal) or [-0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            d3cc05369e2.cif
_cod_data_source_block           s23mkw14
_cod_depositor_comments
'Adding full bibliography for 7132488--7132493.cif.'
_cod_original_formula_sum        'C55.50 H60 B Cl N6 Ni'
_cod_database_code               7132488
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4817(7)
 0.5183(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C56-C53
 1.54 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C56)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H53(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C2(H2), C3(H3), C6(H6A), C8(H8), C15(H15), C17(H17), C23(H23),
  C24(H24), C27(H27), C29(H29), C36(H36), C38(H38), C44(H44), C45(H45),
 C46(H46), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              7508
_shelx_hkl_checksum              12104
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2