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_4326997
_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         'C81 H57 Co3 Cr2 N27 O8, 8(C O), 20(O)'
_chemical_formula_sum            'C89 H57 Co3 Cr2 N27 O36'
_chemical_formula_weight         2361.41
_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                 101.268(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.133(5)
_cell_length_b                   32.248(5)
_cell_length_c                   10.7698(12)
_cell_measurement_reflns_used    2111
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.30
_cell_volume                     12307(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2243
_diffrn_reflns_av_sigmaI/netI    0.1501
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            66150
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.26
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       plate
_exptl_crystal_F_000             4788
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8720
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+40.0147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.3088
_reflns_number_gt                4497
_reflns_number_total             8720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201534e_si_002_2.cif
_cod_data_source_block           1222GuillotICMMO
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4326997