Enhanced Ion Anisotropy by Nonconventional Coordination Geometry: Single-Chain Magnet Behavior for a [{FeIIL}2{NbIV(CN)8}] Helical Chain Compound Designed with Heptacoordinate FeII
Thengarai S. Venkatakrishnan; Shaon Sahoo; Nicolas Bréfuel; Carine Duhayon; Carley Paulsen; Anne-Laure Barra; S. Ramasesha; Jean-Pascal Sutter; Journal of the American Chemical Society 132 (2010) 6047–6056; doi:10.1021/ja9089389

data_4102377
_publ_contact_author_address
; 
Laboratoire de Chimie de Coordination du CNRS, 
205 route de Narbonne, 31077 Toulouse, 
France
;
_publ_contact_author_email       sutter@lcc-toulouse.fr
_publ_contact_author_fax         '(33) 5 61 55 30 03'
_publ_contact_author_name        'Jean-Pascal Sutter'
_publ_contact_author_phone       '(33) 5 61 33 31 57'
_publ_section_title
;
 Enhanced Ion Anisotropy by Nonconventional Coordination Geometry:
 Single-Chain Magnet Behavior for a [{FeIIL}2{NbIV(CN)8}] Helical Chain
 Compound Designed with Heptacoordinate FeII
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6047
_journal_page_last               6056
_journal_paper_doi               10.1021/ja9089389
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C38 H48 Fe2 Mo N18 O, 5(H2 O)'
_chemical_formula_sum            'C38 H58 Fe2 Mo N18 O6'
_chemical_formula_weight         1070.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-04-26
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 99.578(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4352(5)
_cell_length_b                   17.5900(10)
_cell_length_c                   21.0784(8)
_cell_measurement_reflns_used    8928
_cell_measurement_temperature    180
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     4911.9(4)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49352
_diffrn_reflns_theta_full        28.255
_diffrn_reflns_theta_max         32.107
_diffrn_reflns_theta_min         3.028
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'blue green'
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_description       stick
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.46
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4776
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1891
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          0.000577
_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: 
 11.3 -3.86 7.94 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1425
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1123
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4776
_reflns_number_total             4776
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            ja9089389_si_003.cif
_cod_data_source_block           Comp_2
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C38 H58 Fe2 Mo1 N18 O6'
_cod_database_code               4102377