An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and its methyl- and n-octyl-functionalized derivatives
Al Isawi, Wisam A.; Zeller, Matthias; Mezei, Gellert; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 1199–1206; doi:10.1107/S2056989023010101

data_2022953
_publ_section_title
;
 An octanuclear nickel(II) pyrazolate cluster with a cubic Ni8 core and
 its methyl- and n-octyl-functionalized derivatives
;
_journal_coeditor_code           XI2028
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1199
_journal_page_last               1206
_journal_paper_doi               10.1107/S2056989023010101
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac
'(C16 H36 N) (C4 H12 N) [Ni8 (C3 H3 N2)12 (O H)6]'
_chemical_formula_moiety
'C16 H36 N +, C4 H12 N +, C36 H42 N24 Ni8 O6 2-'
_chemical_formula_sum            'C56 H90 N26 Ni8 O6'
_chemical_formula_weight         1693.21
_chemical_name_systematic
;
Tetrabutylazanium tetramethylazanium
hexa-\m~4~-hydroxido-dodeca-\m~2~-pyrazolato-<i>hexahedro</i>-octanickel
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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            2
_cell_length_a                   16.6921(4)
_cell_length_b                   16.6921(4)
_cell_length_c                   12.4112(4)
_cell_measurement_reflns_used    8487
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.4875
_cell_measurement_theta_min      6.9223
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_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2020)
;
_computing_data_collection
;
APEX4 v2021.10-RC6 (Bruker, 2021)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b),
<i>ShelXle</i> Rev1275(H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonIII_C14 charge-integrating and
photon counting pixel array detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10921
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.620
_diffrn_reflns_theta_min         6.921
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    2.863
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.403
_refine_ls_extinction_coef       0.00094(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1094
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0406P)^2^+14.3393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                1052
_reflns_number_total             1094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xi2028sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3458.09(18)
_cod_database_code               2022953
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.612
_shelx_hkl_checksum              55723
_shelx_res_checksum              82379
_cod_database_fobs_code 2022953