Octanuclear Ni(ii) cubes based on halogen-substituted pyrazolates: synthesis, structure, electrochemistry and magnetism
Wang, Zhi; Jagličić, Zvonko; Han, Lu-Lu; Zhuang, Gui-Lin; Luo, Geng-Geng; Zeng, Su-Yuan; Tung, Chen-Ho; Sun, Di; CrystEngComm 18 (2016) 3462–; doi:10.1039/C6CE00528D

data_7224904
_publ_section_title
;
 Octanuclear Ni(ii) cubes based on halogen-substituted pyrazolates:
 synthesis, structure, electrochemistry and magnetism
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3462
_journal_paper_doi               10.1039/C6CE00528D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C48 H62 Br12 N26 Ni8 O6'
_chemical_formula_weight         2527.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.043(6)
_cell_length_b                   22.205(7)
_cell_length_c                   17.844(5)
_cell_measurement_temperature    173(2)
_cell_volume                     8338(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'bruker apex ii'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1408
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40524
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    7.573
_exptl_absorpt_correction_T_max  0.5825
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7313
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1730
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1264P)^2^+3.5939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2527
_reflns_number_gt                3563
_reflns_number_total             7313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00528d2.cif
_cod_data_source_block           p2
_cod_depositor_comments
'Adding full bibliography for 7224903--7224905.cif.'
_cod_database_code               7224904