The curious cases of tetrahydrosalen-type ligands interacting with Ni(II): structures and ligand-based oxidation reactions
Xu, Vivian; Pandey, Bedraj; Jayawardhena, J. P. I. Dulmini; Krause, Jeanette A.; Guan, Hairong; Dalton Transactions  (2023) –; doi:10.1039/D3DT02023A

data_7713624
_publ_section_title
;
 The curious cases of tetrahydrosalen-type ligands interacting with
 Ni(II): structures and ligand-based oxidation reactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02023A
_journal_year                    2023
_chemical_formula_moiety         'C44 H46 N4 O4 Ni,C H Cl3'
_chemical_formula_sum            'C45 H47 Cl3 N4 Ni O4'
_chemical_formula_weight         872.92
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-06-26 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.362(2)
_cell_angle_beta                 92.6794(18)
_cell_angle_gamma                96.6847(18)
_cell_formula_units_Z            4
_cell_length_a                   8.7410(4)
_cell_length_b                   20.9370(13)
_cell_length_c                   23.4276(14)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.28
_cell_volume                     4112.5(4)
_computing_cell_refinement       'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2018.7.2 (Bruker, 2018)'
_computing_data_reduction        'Bruker SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement
'SHELXL-2017/1 (Sheldrick, 2017, G.M. Sheldrick (2015) Acta Cryst., C71, 3-8)'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon-II'
_diffrn_measurement_method       '\w-\f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            221560
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.335
_diffrn_reflns_theta_min         1.996
_diffrn_source                   'Incoatec Mo-microfocus 3.0'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2 (L.Krause, et al. J. Appl. Cryst. (2015), 48, 3-10)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         20498
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0386P)^2^+3.9910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15926
_reflns_number_total             20498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02023a2.cif
_cod_data_source_block           NiHsalophan-Me2_chloroform
_cod_database_code               7713624
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              82630