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_7128995
_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         'C23 H31 N3 Ni O4 S'
_chemical_formula_sum            'C23 H31 N3 Ni O4 S'
_chemical_formula_weight         504.28
_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   geom
_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                90
_cell_angle_beta                 107.073(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4967(19)
_cell_length_b                   12.7673(15)
_cell_length_c                   11.5945(14)
_cell_measurement_reflns_used    4638
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.49
_cell_volume                     2334.4(5)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         1.291
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.745210
_exptl_absorpt_correction_T_min  0.641389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1 - Bruker AXS'
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         7103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1160P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5748
_reflns_number_total             7103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03077a2.cif
_cod_data_source_block           Hardeep2b_0m
_cod_depositor_comments
'Adding full bibliography for 7128990--7128999.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128995
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.781
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              43931
_shelx_hkl_checksum              82170