Synthesis of cubane-type Ni(II) complexes from pyridyl-alcohol ligands; their single-molecule magnet behaviour.
Hameury, Sophie; Kayser, Laure; Pattacini, Roberto; Rogez, Guillaume; Wernsdorfer, Wolfgang; Braunstein, Pierre; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5013–5024; doi:10.1039/c3dt32869d

data_7023848
_publ_section_title
;
 Synthesis of cubane-type Ni(II) complexes from pyridyl-alcohol ligands;
 their single-molecule magnet behaviour.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5013
_journal_page_last               5024
_journal_paper_doi               10.1039/c3dt32869d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C36 H56 Cl4 N4 Ni4 O8, 3(C H2 Cl2) '
_chemical_formula_sum            'C39 H62 Cl10 N4 Ni4 O8'
_chemical_formula_weight         1304.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.868(2)
_cell_angle_beta                 72.476(2)
_cell_angle_gamma                72.690(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8999(4)
_cell_length_b                   13.8702(4)
_cell_length_c                   16.8384(6)
_cell_measurement_reflns_used    7198
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2734.94(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18588
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         12454
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                8232
_reflns_number_total             12454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32869d.txt
_cod_data_source_block           compound5
_cod_original_cell_volume        2734.94(15)
_cod_database_code               7023848