Square-planar and octahedral nickel complexes of an acylhydrazone ligand and the serendipitous isolation of a potential octahedral nickel acylhydrazone precursor
Carballo, Rosa; Lago, Ana Belén; Vázquez-Toirán, María; Estévez, Laura; Vázquez-López, Ezequiel M.; CrystEngComm 25 (2023) 2463–2472; doi:10.1039/D3CE00160A

data_7246511
_publ_section_title
;
 Square-planar and octahedral nickel complexes of an acylhydrazone ligand
 and the serendipitous isolation of a potential octahedral nickel
 acylhydrazone precursor
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2463
_journal_page_last               2472
_journal_paper_doi               10.1039/D3CE00160A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C28 H26 N4 Ni O8'
_chemical_formula_weight         605.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-12-19 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.289(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6680(18)
_cell_length_b                   5.9629(5)
_cell_length_c                   23.892(2)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.97
_cell_volume                     2865.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.471
_diffrn_reflns_theta_min         2.353
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.184
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3583
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0515P)^2^+15.1807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2885
_reflns_number_total             3583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00160a2.cif
_cod_data_source_block           2A-32010103_0m
_cod_depositor_comments
'Adding full bibliography for 7246508--7246511.cif.'
_cod_original_cell_volume        2865.7(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7246511
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.877
_shelx_res_checksum              10241
_shelx_hkl_checksum              3128