Stepwise Formation of a Pentanuclear Ni4Cu Heterometallic Complex Exhibiting a Vertex-Sharing Defective Double-Cubane Core and Diphenoxo- and Phenoxo/Azide Bridging Groups: A Magnetostructural and DFT Theoretical Study
Koushik Pramanik; Pijush Malpaharia; Antonio J. Mota; Enrique Colacio; Babulal Das; F. Lloret; Swapan K. Chandra; Inorganic Chemistry 52 (2013) 3995–4001; doi:10.1021/ic302784q

data_4334348
_publ_section_title
;
 Stepwise Formation of a Pentanuclear Ni4Cu Heterometallic Complex
 Exhibiting a Vertex-Sharing Defective Double-Cubane Core and Diphenoxo-
 and Phenoxo/Azide Bridging Groups: A Magnetostructural and DFT
 Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3995
_journal_page_last               4001
_journal_paper_doi               10.1021/ic302784q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C64 H76 Cl2 Cu N16 Ni4 O16'
_chemical_formula_weight         1694.69
_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                97.109(4)
_cell_angle_beta                 95.005(4)
_cell_angle_gamma                118.087(4)
_cell_formula_units_Z            1
_cell_length_a                   12.1130(9)
_cell_length_b                   12.7063(9)
_cell_length_c                   13.1498(9)
_cell_measurement_temperature    296(2)
_cell_volume                     1747.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13461
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       blocks
_exptl_crystal_F_000             875
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         5913
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                3047
_reflns_number_total             5913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302784q_si_002.cif
_cod_data_source_block           compound1
_cod_database_code               4334348