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_7132492
_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         'C53 H59 B N6 Ni'
_chemical_formula_sum            'C57 H69 B N6 Ni O'
_chemical_formula_weight         923.70
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-29 deposited with the CCDC.	2023-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.618(2)
_cell_angle_beta                 84.570(2)
_cell_angle_gamma                75.422(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4827(3)
_cell_length_b                   15.0976(4)
_cell_length_c                   15.7441(5)
_cell_measurement_reflns_used    12100
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0890
_cell_measurement_theta_min      4.2520
_cell_volume                     2625.77(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.316
_diffrn_reflns_theta_min         3.990
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         10494
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0575P)^2^+0.3325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8795
_reflns_number_total             10494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05369e2.cif
_cod_data_source_block           s23mkw46
_cod_depositor_comments
'Adding full bibliography for 7132488--7132493.cif.'
_cod_database_code               7132492
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C43-H43A = C43-H43C = C43-H43B
 0.98 with sigma of 0.005
3.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C38(H38), C23(H23), C2(H2), C15(H15), C17(H17), C24(H24),
 C36(H36), C3(H3), C8(H8), C27(H27), C45(H45), C29(H29), C46(H46), C51(H51),
 C6(H6A), C47(H47), C53(H53), C52(H52)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C12(H12A,H12B,H12C), C19(H19A,
 H19B,H19C), C41(H41A,H41B,H41C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28898
_shelx_hkl_checksum              72654
_shelx_fab_checksum              53897
_olex2_submission_special_instructions 'No special instructions were received'