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_7711930
_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         'C16 H26 Br Cl N Ni O P'
_chemical_formula_sum            'C16 H26 Br Cl N Ni O P'
_chemical_formula_weight         453.42
_chemical_name_systematic
'[{\kP,\kC-(i-Pr)2PO-(5-Cl-C6H3)}{\kN-(CH3CH2-)(CH3CH=)N}Ni(Br)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2022-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                85.083(2)
_cell_angle_beta                 83.391(3)
_cell_angle_gamma                89.300(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1691(4)
_cell_length_b                   10.6197(5)
_cell_length_c                   11.5954(5)
_cell_measurement_reflns_used    6863
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.643
_cell_measurement_theta_min      4.178
_cell_volume                     995.58(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1273
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26093
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.221
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    5.748
_exptl_absorpt_correction_T_max  0.679080
_exptl_absorpt_correction_T_min  0.383360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1582 before and 0.0553 after correction.
 
For component 2:
 wR2(int) was 0.1851 before and 0.0722 after correction.
 The Ratio of minimum to maximum transmission is 0.56.

Final HKLF 4 output contains 26093 reflections, Rint = 0.1273
 (16121 with I > 3sig(I), Rint = 0.1210)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       Block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+1.4523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             3767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02979k2.cif
_cod_data_source_block           rajib38
_cod_depositor_comments
'Adding full bibliography for 7711929--7711939.cif.'
_cod_database_code               7711930
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.494
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.72149
 0.27851
2.a Ternary CH refined with riding coordinates:
 C11(H11), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C3(H3), C14(H14)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C),
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              35244
_olex2_submission_special_instructions 'No special instructions were received'