Structural and magnetic variations in tetranuclear Ni(II) clusters: the effect of the reaction solvent and ligand substitution on product identity.
Perlepe, Panagiota S.; Athanasopoulou, Angeliki A.; Alexopoulou, Konstantina I.; Raptopoulou, Catherine P.; Psycharis, Vassilis; Escuer, Albert; Perlepes, Spyros P.; Stamatatos, Theocharis C.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16605–16609; doi:10.1039/c4dt02434f

data_7032641
_publ_section_title
;
 Structural and magnetic variations in tetranuclear Ni(II) clusters: the
 effect of the reaction solvent and ligand substitution on product
 identity.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16605
_journal_page_last               16609
_journal_paper_doi               10.1039/c4dt02434f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C68 H72 N8 Ni4 O12'
_chemical_formula_weight         1428.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                63.7240(10)
_cell_angle_beta                 82.2820(10)
_cell_angle_gamma                81.8030(10)
_cell_formula_units_Z            1
_cell_length_a                   11.3987(2)
_cell_length_b                   11.9871(2)
_cell_length_c                   12.9916(2)
_cell_measurement_reflns_used    18186
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.83
_cell_measurement_theta_min      6.73
_cell_volume                     1570.38(5)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21294
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.73
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0583P)^2^+0.5879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                4022
_reflns_number_total             5057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02434f2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7032640--7032642.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7032641