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_7132491
_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         'C42 H48 N4 Ni2, C12 H8 B O4'
_chemical_formula_sum            'C55.2 H57 B F0.2 N4 Ni2 O4'
_chemical_formula_weight         972.47
_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     dual
_audit_creation_date             2023-06-06
_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                91.823(3)
_cell_angle_beta                 99.146(3)
_cell_angle_gamma                97.973(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0673(3)
_cell_length_b                   13.4580(5)
_cell_length_c                   15.2235(5)
_cell_measurement_reflns_used    8998
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.1050
_cell_measurement_theta_min      4.3730
_cell_volume                     2413.63(14)
_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      150.01(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  0.0368
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27223
_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         73.221
_diffrn_reflns_theta_min         3.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82193
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             1022
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9612
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0493P)^2^+0.7919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7610
_reflns_number_total             9612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05369e2.cif
_cod_data_source_block           s23mkw50
_cod_depositor_comments
'Adding full bibliography for 7132488--7132493.cif.'
_cod_original_cell_volume        2413.62(14)
_cod_original_formula_sum        'C55.20 H57 B F0.20 N4 Ni2 O4'
_cod_database_code               7132491
_shelx_shelxl_version_number     2019/3
_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. Restrained distances
 N4-C25 \\sim N4-C25A
 with sigma of 0.005
 C32-C28 \\sim C32A-C28A \\sim C33A-C26A \\sim C33-C26 \\sim C31-C30 \\sim
C31A-C30A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26 \\sim C31 \\sim C32 \\sim
C33 \\sim C25A \\sim C30A \\sim C29A \\sim C28A \\sim C27A \\sim C26A \\sim
C31A \\sim C32A \\sim C33A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.01 within 2A
Uanis(C26) = Uanis(C26A)
4. Others
 Fixed Sof: C25(0.65) C30(0.65) C29(0.65) H29(0.65) C28(0.65) C27(0.65)
 H27(0.65) C26(0.65) C31(0.65) H31A(0.65) H31B(0.65) H31C(0.65) C32(0.65)
 H32A(0.65) H32B(0.65) H32C(0.65) C33(0.65) H33A(0.65) H33B(0.65) H33C(0.65)
 C25A(0.35) C30A(0.35) C29A(0.35) H29A(0.35) C28A(0.35) C27A(0.35) H27A(0.35)
 C26A(0.35) C31A(0.35) H31D(0.35) H31E(0.35) H31F(0.35) C32A(0.35) H32D(0.35)
 H32E(0.35) H32F(0.35) C33A(0.35) H33D(0.35) H33E(0.35) H33F(0.35)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24),
 C36(H36), C38(H38), C29(H29), C27(H27), C29A(H29A), C27A(H27A), C45(H45),
 C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54)
5.b Fitted hexagon refined as free rotating group:
 C25(C30,C29,C28,C27,C26), C25A(C30A,C29A,C28A,C27A,C26A)
5.c 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), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C33A(H33D,
 H33E,H33F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12227
_shelx_hkl_checksum              9718
_shelx_fab_checksum              2823
_olex2_submission_special_instructions 'No special instructions were received'