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_7032640
_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            'C65.4 H72.2 N4 Ni4 O12.7'
_chemical_formula_weight         1352.31
_chemical_name_systematic
; 
 ? 
;
_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                94.7490(10)
_cell_angle_beta                 95.5530(10)
_cell_angle_gamma                105.1460(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0042(2)
_cell_length_b                   14.6854(3)
_cell_length_c                   18.3859(3)
_cell_measurement_reflns_used    28122
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.95
_cell_measurement_theta_min      6.56
_cell_volume                     3094.15(10)
_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 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36381
_diffrn_reflns_theta_full        64.00
_diffrn_reflns_theta_max         64.00
_diffrn_reflns_theta_min         6.56
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         9690
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+1.9583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                7126
_reflns_number_total             9690
_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_original_formula_sum        'C65.40 H72.20 N4 Ni4 O12.70'
_cod_database_code               7032640