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_7711934
_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         'C17 H29 Br N Ni O2 P'
_chemical_formula_sum            'C17 H29 Br N Ni O2 P'
_chemical_formula_weight         449.00
_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             2022-08-10
_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                87.918(2)
_cell_angle_beta                 86.659(2)
_cell_angle_gamma                74.060(2)
_cell_formula_units_Z            4
_cell_length_a                   8.7051(4)
_cell_length_b                   10.5840(5)
_cell_length_c                   22.8298(11)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.660
_cell_measurement_theta_min      3.780
_cell_volume                     2018.65(17)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41903
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.836
_diffrn_reflns_theta_min         3.375
_diffrn_source_current           2.85
_diffrn_source_power             0.19921500000000003
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    7.316
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.3491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1687 before and 0.1060 after correction.
The Ratio of minimum to maximum transmission is 0.4643.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9162
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7430
_reflns_number_total             9162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02979k2.cif
_cod_data_source_block           rajib271
_cod_depositor_comments
'Adding full bibliography for 7711929--7711939.cif.'
_cod_database_code               7711934
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17B-C16B \\sim C14A-C15A \\sim C15B-C14B \\sim C17A-C16A
 with sigma of 0.02
 C31A-C32A \\sim C31B-C32B \\sim C33A-C34A \\sim C33B-C34B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16B \\sim C16A \\sim C14A \\sim C14B: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
C15A \\sim C15B \\sim C17B \\sim C17A: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
C31B \\sim C31A \\sim C33A \\sim C33B: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
C32A \\sim C32B \\sim C34A \\sim C34B: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
4. Others
 Sof(C16B)=Sof(H16B)=Sof(C14B)=Sof(H14B)=Sof(H14C)=Sof(C17B)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C34B)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C33B)=Sof(H33B)=Sof(H33C)=Sof(C31B)=
 Sof(H31C)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C14A)=Sof(H14A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C16A)=Sof(H16A)=Sof(H16C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C25(H25), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C14B(H14B,H14C), C16A(H16A,H16C), C33B(H33B,H33C)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C3(H3), C20(H20), C21(H21), C23(H23), C16B(H16B), C14A(H14A),
 C33A(H33A), C31B(H31C)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C7(H7A,H7B,
 H7C), C9(H9A,H9B,H9C), C15A(H15A,H15B,H15C), C17A(H17A,H17B,H17C), C30(H30A,
 H30B,H30C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C32A(H32A,H32B,H32C),
 C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C34A(H34A,H34B,H34C), C17B(H17D,H17E,
 H17F), C15B(H15D,H15E,H15F), C34B(H34D,H34E,H34F), C32B(H32D,H32E,H32F)
;
_shelx_res_checksum              38298
_olex2_submission_special_instructions 'No special instructions were received'