Pentanuclear Cyanide-Bridged Complexes Based on Highly Anisotropic CoII Seven-Coordinate Building Blocks: Synthesis, Structure, and Magnetic Behavior
Luke J. Batchelor; Marco Sangalli; Régis Guillot; Nathalie Guihéry; Remi Maurice; Floriana Tuna; Talal Mallah; Inorganic Chemistry 50 (2011) 12045–12052; doi:10.1021/ic201534e

data_4326998
_publ_contact_author_address
;Institut de Chimie Mol\'eculaire et des Mat\'eriaux d?Orsay,
UMR8182,
CNRS, 
Universit\'e Paris-Sud 11, 
91405 Orsay,
France.
;
_publ_contact_author_email       talal.mallah@u-psud.fr
_publ_contact_author_fax         '(+33) 1 69 15 47 54'
_publ_contact_author_name        'Luke Batchelor'
_publ_contact_author_phone       '(+33) 1 69 15 47 49'
_publ_section_title
;
 Pentanuclear Cyanide-Bridged Complexes Based on Highly Anisotropic CoII
 Seven-Coordinate Building Blocks: Synthesis, Structure, and Magnetic
 Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12045
_journal_page_last               12052
_journal_paper_doi               10.1021/ic201534e
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C811 H67 Co3 Fe2 N27 O8, 18(H2 O)'
_chemical_formula_sum            'C81 H103 Co3 Fe2 N27 O26'
_chemical_formula_weight         2159.39
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 95.861(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.312(2)
_cell_length_b                   16.7668(9)
_cell_length_c                   17.1653(10)
_cell_measurement_temperature    100(1)
_cell_volume                     9537.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75638
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.8496
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         15835
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.159
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+14.4050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                11110
_reflns_number_total             15835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201534e_si_002_3.cif
_cod_data_source_block           1234GuillotICMMO
_cod_original_cell_volume        9537.5(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326998