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_7132493
_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         'C48 H52 B Cl N4 Ni O2, 1(C6 D6)'
_chemical_formula_sum            'C54 H52 B Cl D6 N4 Ni O2'
_chemical_formula_weight         906.05
_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     direct
_audit_creation_date             2022-08-08
_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                 96.737(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.482(4)
_cell_length_b                   13.929(5)
_cell_length_c                   33.577(13)
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.242
_cell_measurement_theta_min      2.344
_cell_volume                     4869(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex III, Bruker'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1452
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            171407
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         1.221
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0777 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.8623.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         11177
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0688P)^2^+10.6167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7534
_reflns_number_total             11177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05369e2.cif
_cod_data_source_block           ilb3953_2_0m
_cod_depositor_comments
'Adding full bibliography for 7132488--7132493.cif.'
_cod_original_cell_volume        4868(3)
_cod_database_code               7132493
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.849
_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. Rigid bond restraints
 C49A, C50A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C49B, C50B, C51B, C52B, C53B, C54B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim C54A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C49B \\sim C50B \\sim C51B \\sim C52B \\sim C53B \\sim C54B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C49B, C50B, C51B, C52B, C53B, C54B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49A, C50A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C53B)=Sof(D53B)=Sof(C54B)=Sof(D54B)=Sof(C49B)=Sof(D49B)=Sof(C50B)=
 Sof(D50B)=Sof(C51B)=Sof(D51B)=Sof(C52B)=Sof(D52B)=1-FVAR(1)
 Sof(C51A)=Sof(D51A)=Sof(C52A)=Sof(D52A)=Sof(C53A)=Sof(D53A)=Sof(C54A)=
 Sof(D54A)=Sof(C49A)=Sof(D49A)=Sof(C50A)=Sof(D50A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C14(H14), C21(H21),
 C23(H23), C29(H29), C30(H30), C33(H33), C35(H35), C42(H42), C44(H44),
 C51A(D51A), C52A(D52A), C53A(D53A), C54A(D54A), C49A(D49A), C50A(D50A),
 C53B(D53B), C54B(D54B), C49B(D49B), C50B(D50B), C51B(D51B), C52B(D52B)
6.b Fitted hexagon refined as free rotating group:
 C51A(C52A,C53A,C54A,C49A,C50A), C53B(C54B,C49B,C50B,C51B,C52B)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              11241
_shelx_hkl_checksum              62747
_olex2_submission_special_instructions 'No special instructions were received'