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_7246509
_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            'C26 H21.06 N4 Ni0.5 O3'
_chemical_formula_weight         466.88
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   34.338(2)
_cell_length_b                   34.338(2)
_cell_length_c                   12.6009(11)
_cell_measurement_reflns_used    5224
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0990
_cell_measurement_theta_min      2.11
_cell_volume                     12867.1(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28739
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.225
_diffrn_reflns_theta_min         3.810
_exptl_absorpt_coefficient_mu    0.886
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Numerical absorption correction based on gaussian integration over 
   a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4375
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5673
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1215P)^2^+7.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3799
_reflns_number_total             5673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00160a2.cif
_cod_data_source_block           3_sq
_cod_depositor_comments
'Adding full bibliography for 7246508--7246511.cif.'
_cod_original_cell_volume        12867(2)
_cod_original_formula_sum        'C26 H21.06 N4 Ni0.50 O3'
_cod_database_code               7246509
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              66218
_shelx_hkl_checksum              69636
_shelx_fab_checksum              17111