Reactivities of cyclonickellated complexes with hydroxylamines: formation of κ<sup>O</sup>-hydroxylamine and κ<sup>N</sup>-imine adducts and a κ<sup>O</sup>, κ<sup>N</sup>-aminoxide derivative.
Sarker, Rajib K.; Mangin, Loïc P; Zargarian, Davit; Dalton transactions (Cambridge, England : 2003) 52 (2023) 366–375; doi:10.1039/d2dt02979k

data_7711939
_publ_section_title
;
 Reactivities of cyclonickellated complexes with hydroxylamines: formation
 of &#x3ba;<sup>O</sup>-hydroxylamine and &#x3ba;<sup>N</sup>-imine
 adducts and a &#x3ba;<sup>O</sup>, &#x3ba;<sup>N</sup>-aminoxide
 derivative.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              366
_journal_page_last               375
_journal_paper_doi               10.1039/d2dt02979k
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C28 H47 Br N2 Ni O2 P2'
_chemical_formula_sum            'C28 H47 Br N2 Ni O2 P2'
_chemical_formula_weight         644.23
_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             2022-05-25
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;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-11 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                91.2360(10)
_cell_angle_beta                 93.385(2)
_cell_angle_gamma                90.311(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6766(3)
_cell_length_b                   10.8198(4)
_cell_length_c                   16.2208(6)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.599
_cell_measurement_theta_min      2.375
_cell_volume                     1519.75(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36465
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.728
_diffrn_reflns_theta_min         2.374
_diffrn_source_current           2.86
_diffrn_source_power             0.199771
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.295
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1510 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8831.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_recrystallization_method 'slow evaporation of Et2O'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0052(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0398P)^2^+0.5297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6672
_reflns_number_total             6953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02979k2.cif
_cod_data_source_block           loic123
_cod_depositor_comments
'Adding full bibliography for 7711929--7711939.cif.'
_cod_database_code               7711939
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.677
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C23(H23), C26(H26)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C16(H16), C17(H17), C18(H18), C20(H20)
1.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              13714
_olex2_submission_special_instructions 'No special instructions were received'