Reversible Solvatomagnetic Effect in Novel Tetranuclear Cubane-Type Ni4 Complexes and Magnetostructural Correlations for the [Ni4(μ3-O)4] Core
Animesh Das; Felix J. Klinke; Serhiy Demeshko; Steffen Meyer; Sebastian Dechert; Franc Meyer; Inorganic Chemistry 51 (2012) 8141–8149; doi:10.1021/ic300535d

data_4329815
_publ_contact_author_address
; Institut f\"ur Anorganische Chemie
  Georg August Universit\"at G\"ottingen
  Tammannstra\&se 4
  D-37077 G\"ottingen
  Germany
;
_publ_contact_author_email       franc.meyer@chemie.uni-goettingen.de
_publ_contact_author_fax         49(551)393063
_publ_contact_author_name        'Prof. Dr. Franc Meyer'
_publ_contact_author_phone       49(551)393012
_publ_section_title
;
 Reversible Solvatomagnetic Effect in Novel Tetranuclear Cubane-Type Ni4
 Complexes and Magnetostructural Correlations for the [Ni4(\m3-O)4] Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8141
_journal_page_last               8149
_journal_paper_doi               10.1021/ic300535d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C48 H56 N8 Ni4 O12, O'
_chemical_formula_sum            'C48 H56 N8 Ni4 O13'
_chemical_formula_weight         1187.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8120(7)
_cell_length_b                   16.8120(7)
_cell_length_c                   17.5449(9)
_cell_measurement_reflns_used    44432
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      1.68
_cell_volume                     4958.9(4)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44432
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         44432
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                23704
_reflns_number_total             44432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300535d_si_002_2.cif
_cod_data_source_block           ad35-1xH2O
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4329815