Synthesis, magnetic properties, and STM spectroscopy of an unprecedented octanuclear chloro-bridged nickel(ii) double cubane.
Scheurer, Andreas; Gieb, Klaus; Alam, Mohammad S.; Heinemann, Frank W.; Saalfrank, Rolf W.; Kroener, Wolfgang; Petukhov, Konstantin; Stocker, Michael; Müller, Paul; Dalton transactions (Cambridge, England : 2003) 41 (2012) 3553–3561; doi:10.1039/c2dt12007k

data_7018473
_publ_section_title
;
 Synthesis, magnetic properties, and STM spectroscopy of an unprecedented
 octanuclear chloro-bridged nickel(ii) double cubane.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3553
_journal_page_last               3561
_journal_paper_doi               10.1039/c2dt12007k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C48 H110 Cl8 N6 Ni8 O14, 4(C H2 Cl2)'
_chemical_formula_sum            'C52 H118 Cl16 N6 Ni8 O14'
_chemical_formula_weight         2088.40
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom except O bound hydrogens difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.408(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2919(14)
_cell_length_b                   19.8972(5)
_cell_length_c                   23.2951(11)
_cell_measurement_reflns_used    420
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     8387.3(8)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
\f- and \w-rotations with 1.40 \% and 84 sec per frame
;
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            98003
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         17683
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+19.5457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                12606
_reflns_number_total             17683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12007k.txt
_cod_data_source_block           rs0804
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7018473