Intramolecular H-bond stabilization of a primary hydroxylamine in salen-type metal complexes.
Singh, Hardeep; MacKay, Alyson; Sheibany, Nooshin; Chen, Fei; Mosser, Maëlle; Rouet, Pierre-Étienne; Rousseau, Frédéric; Askari, Mohammad S.; Ottenwaelder, Xavier; Chemical communications (Cambridge, England) 57 (2021) 10403–10406; doi:10.1039/d1cc03077a

data_7128991
_publ_section_title
;
 Intramolecular H-bond stabilization of a primary hydroxylamine in
 salen-type metal complexes.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10403
_journal_page_last               10406
_journal_paper_doi               10.1039/d1cc03077a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C15 H15 N3 Ni O3 S, 0.5 (H2 O)'
_chemical_formula_sum            'C15 H16 N3 Ni O3.5 S'
_chemical_formula_weight         385.08
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-06-07 deposited with the CCDC.	2021-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                98.838(4)
_cell_angle_beta                 112.789(4)
_cell_angle_gamma                108.273(4)
_cell_formula_units_Z            4
_cell_length_a                   11.9552(9)
_cell_length_b                   12.1760(9)
_cell_length_c                   12.7970(9)
_cell_measurement_reflns_used    8338
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      3.95
_cell_volume                     1548.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.930
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20646
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.802
_diffrn_reflns_theta_min         3.947
_exptl_absorpt_coefficient_mu    3.274
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0375
_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^)+3.7283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4556
_reflns_number_total             5327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03077a2.cif
_cod_data_source_block           Hardeep4_0m
_cod_depositor_comments
'Adding full bibliography for 7128990--7128999.cif.'
_cod_original_formula_sum        'C15 H16 N3 Ni O3.50 S'
_cod_database_code               7128991
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              42324
_shelx_hkl_checksum              27297