A family of cubane cobalt and nickel clusters: Syntheses, structures and magnetic properties
Shu-Hua Zhang; Yi Dong Zhang; Hua Hong Zou; Jing Jing Guo; He Ping Li; You Song; Hong Liang; Inorganica Chimica Acta 396 (2013) 119–125; doi:10.1016/j.ica.2012.10.032

data_1513001
_publ_section_title
;
 A family of cubane cobalt and nickel clusters: Syntheses, structures and
 magnetic properties
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              119
_journal_page_last               125
_journal_paper_doi               10.1016/j.ica.2012.10.032
_journal_volume                  396
_journal_year                    2013
_chemical_formula_sum            'C36 H40 Cl8 Ni4 O16'
_chemical_formula_weight         1247.12
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.927(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6063(14)
_cell_length_b                   44.885(6)
_cell_length_c                   11.7452(17)
_cell_measurement_temperature    173(2)
_cell_volume                     4869.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12156
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.5634
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7383
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+25.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                6390
_reflns_number_total             7383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-396-119-125-5.cif
_cod_data_source_block           ni1
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1513001