Condensation of a Nickel Tetranuclear Cubane into a Heptanuclear Single-Molecule Magnet
Sarah Petit; Petr Neugebauer; Guillaume Pilet; Guillaume Chastanet; Anne-Laure Barra; Arlei B. Antunes; Wolfgang Wernsdorfer; Dominique Luneau; Inorganic Chemistry 51 (2012) 6645–6654; doi:10.1021/ic3001637

data_4329452
_publ_section_title
;
 Condensation of a Nickel Tetranuclear Cubane into a Heptanuclear
 Single-Molecule Magnet
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6645
_journal_page_last               6654
_journal_paper_doi               10.1021/ic3001637
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C70 H54 F36 N8 Ni7 O20'
_chemical_formula_sum            'C70 H54 F36 N8 Ni7 O20'
_chemical_formula_weight         2422.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 91.703(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.705(3)
_cell_length_b                   18.746(16)
_cell_length_c                   21.701(7)
_cell_measurement_reflns_used    10255
_cell_measurement_temperature    293
_cell_measurement_theta_max      28
_cell_measurement_theta_min      0
_cell_volume                     5166(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.090
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11133
_diffrn_reflns_theta_full        25.219
_diffrn_reflns_theta_max         28.658
_diffrn_reflns_theta_min         1.436
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.9323
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.93
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1488
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         4627
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.1593
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.003107
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.89 0.822 1.30 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1441
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0884
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                4627
_reflns_number_total             10782
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0801
_oxford_refine_ls_scale          0.2322(8)
_oxford_reflns_number_all        10731
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ic3001637_si_001_2.cif
_cod_data_source_block           '[Ni7]'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4329452