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_7711937
_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         'C21 H32 Br0.717 Cl0.283 N2 Ni O2 P'
_chemical_formula_sum            'C21 H32 Br0.7 Cl0.3 N2 Ni O2 P'
_chemical_formula_weight         500.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.918(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5518(11)
_cell_length_b                   10.3023(5)
_cell_length_c                   10.8188(7)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.86
_cell_measurement_theta_min      4.81
_cell_volume                     2268.8(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4343
_diffrn_reflns_point_group_measured_fraction_full 0.492
_diffrn_reflns_point_group_measured_fraction_max 0.481
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.555
_diffrn_reflns_theta_min         2.170
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  0.753552
_exptl_absorpt_correction_T_min  0.583658
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1254 before and 0.0678 after correction.
 
For component 2:
 wR2(int) was 0.1348 before and 0.0658 after correction.
 The Ratio of minimum to maximum transmission is 0.78.

Final HKLF 4 output contains 40178 reflections, Rint = 0.0746
 (25708 with I > 3sig(I), Rint = 0.0677)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         4343
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0516
_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^)+(0.1230P)^2^+0.6199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                4149
_reflns_number_total             4343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02979k2.cif
_cod_data_source_block           rajib51
_cod_depositor_comments
'Adding full bibliography for 7711929--7711939.cif.'
_cod_original_formula_sum        'C21 H32 Br0.70 Cl0.30 N2 Ni O2 P'
_cod_database_code               7711937
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5758
 0.4242
2. Restrained distances
 Ni2-Cl2
 2.22 with sigma of 0.005
 Br2-Ni2
 2.35 with sigma of 0.005
 Ni1-Cl1
 2.22 with sigma of 0.001
 Br1-Ni1
 2.35 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Br2)
Uanis(Cl1) = Uanis(Br1)
4. Rigid body (RIGU) restrains
 C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
 Sof(Cl1)=1-FVAR(2)
 Sof(Br1)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C30(H30), C33(H33)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C15(H15A,H15B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C24(H24), C25(H25), C27(H27), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43)
6.d 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), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              4899
_olex2_submission_special_instructions 'No special instructions were received'