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_7711938
_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         'C18 H32 Br N2 Ni O P'
_chemical_formula_sum            'C18 H32 Br N2 Ni O P'
_chemical_formula_weight         462.04
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 130.3570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.6233(12)
_cell_length_b                   8.5715(4)
_cell_length_c                   21.7605(15)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.105
_cell_measurement_theta_min      2.986
_cell_volume                     4210.4(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEX2 CCD'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41086
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.098
_diffrn_reflns_theta_min         3.916
_diffrn_source_current           0.65
_diffrn_source_power             0.029119999999999997
_diffrn_source_voltage           44.8
_exptl_absorpt_coefficient_mu    4.319
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.6726.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+4.3171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3916
_reflns_number_total             3962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02979k2.cif
_cod_data_source_block           rajib4
_cod_depositor_comments
'Adding full bibliography for 7711929--7711939.cif.'
_cod_database_code               7711938
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H17B,H17C} of C17B, {H15A,H15B} of C15A
 At 1.5 times of:
  All C(H,H,H) groups, {H14A,H14B} of C14
2. Restrained distances
 C15A-C16A \\sim C17B-C18B
 with sigma of 0.02
 C15B-C16B \\sim C17A-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15A \\sim C15B \\sim C17A \\sim C17B: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
C16B \\sim C16A \\sim C18B \\sim C18A: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1A
4. Others
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17B)=Sof(H17B)=Sof(H17C)=
 Sof(C15B)=Sof(H15C)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15A)=
 Sof(H15A)=Sof(H15B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C17B(H17B,H17C)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C17A(H17A), C15B(H15C)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C16A(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C18B(H18D,
 H18E,H18F), C16B(H16D,H16E,H16F)
;
_shelx_res_checksum              56108
_olex2_submission_special_instructions 'No special instructions were received'