Reactions of cyclonickelated complexes with hydroxylamines and TEMPO˙: isolation of new TEMPOH adducts of Ni(II) and their reactivities with nucleophiles and oxidants.
Sarker, Rajib K.; Zargarian, Davit; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10208–10219; doi:10.1039/d4dt00605d

data_7716237
_publ_section_title
;
 Reactions of cyclonickelated complexes with hydroxylamines and
 TEMPO&#x2d9;: isolation of new TEMPOH adducts of Ni(II) and their
 reactivities with nucleophiles and oxidants.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10208
_journal_page_last               10219
_journal_paper_doi               10.1039/d4dt00605d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H39 Br0.25 Cl0.75 N Ni O3 P'
_chemical_formula_sum            'C22 H39 Br0.25 Cl0.75 N Ni O3 P'
_chemical_formula_weight         501.78
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-06 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.950(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9270(5)
_cell_length_b                   14.1466(6)
_cell_length_c                   29.5812(12)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    150
_cell_measurement_theta_max      54.862
_cell_measurement_theta_min      2.632
_cell_volume                     4930.4(4)
_computing_cell_refinement
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 3 (2019) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2020) V8.40B; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'Bruker CMOS Photon III '
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45605
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.923
_diffrn_reflns_theta_min         2.631
_diffrn_source                   'Metal Jet'
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    5.623
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.7702.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9244
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0366P)^2^+2.3477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8631
_reflns_number_total             9244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00605d2.cif
_cod_data_source_block           rajib901
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716231--7716238.cif.
;
_cod_database_code               7716237
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.557
_shelx_estimated_absorpt_t_min   0.434
_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
 Cl2-Ni2 \\sim Cl1-Ni1
 with sigma of 0.02
 Br2-Ni2 \\sim Br1-Ni1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Br1 \\sim Cl1 \\sim Br2 \\sim Cl2: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1A
Uanis(Cl2) = Uanis(Br2)
Uanis(Br1) = Uanis(Cl1)
4. Others
 Fixed Sof: Br1(0.25) Cl1(0.75) Br2(0.25) Cl2(0.75)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C30(H30), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C25(H25), C26(H26), C28(H28)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              94529
_olex2_submission_special_instructions 'No special instructions were received'