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_7246510
_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            'C34 H40 N4 Ni O9'
_chemical_formula_weight         707.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 99.623(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8040(10)
_cell_length_b                   18.8611(14)
_cell_length_c                   16.7162(14)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.44
_cell_volume                     3358.4(5)
_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 0.998
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62044
_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         2.358
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.104
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00091(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0341P)^2^+7.5938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7048
_reflns_number_total             8361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00160a2.cif
_cod_data_source_block           2B-32010101_0m
_cod_depositor_comments
'Adding full bibliography for 7246508--7246511.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7246510
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              4700
_shelx_hkl_checksum              43826