A tetranuclear nickel(II) complex, [Ni4(L)4](ClO4)4·C2H3N·2H2O, with an asymmetric Ni4O4 open-cubane-like core
Patel, R. N.; Patel, S. K.; Patel, A. K.; Patel, N.; Butcher, Ray J.; Acta Crystallographica Section E Crystallographic Communications 78 (2022) –; doi:10.1107/S2056989021012408

data_2022514
_publ_section_title
;
 A tetranuclear nickel(II) complex,
 [Ni4(L)4](ClO4)4&#x00B7;C2H3N&#x00B7;2H2O, with an asymmetric Ni4O4
 open-cubane-like core
;
_journal_coeditor_code           YY2002
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989021012408
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_iupac
'[Ni4 (C13 H12 N3 O2)4] (Cl O4)4, C2 H3 N, 2H2 O'
_chemical_formula_moiety
;
C52 H48 N12 Ni4 O8, 4(Cl O4), C2 H3 N, 2(H2 O)
;
_chemical_formula_sum            'C54 H55 Cl4 N13 Ni4 O26'
_chemical_formula_weight         1678.75
_chemical_name_systematic
;<i>cyclo</i>-Tetrakis(\m-2-methoxy-6-{[2-(pyridin-2-yl)hydrazin-1-ylidene]methyl}phenolato)tetranickel(II) tetrakis(perchlorate) acetonitrile
monosolvate dihydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5976(6)
_cell_length_b                   11.8723(3)
_cell_length_c                   22.2989(6)
_cell_measurement_reflns_used    9461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.43
_cell_volume                     6247.2(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86241
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.920
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       needle
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.299
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4529 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.024(5)
_refine_ls_extinction_coef       0.00135(19)
_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   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         14617
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0571P)^2^+9.1783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                11629
_reflns_number_total             14617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yy2002sup1.cif
_cod_data_source_block           I
_cod_database_code               2022514
_shelx_hkl_checksum              82644
_shelx_res_checksum              37631
_cod_database_fobs_code 2022514