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_4102378
_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 N18 O W, 3.5(H2 O) '
_chemical_formula_sum            'C38 H55 Fe2 N18 O4.5 W'
_chemical_formula_weight         1131.52
_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             07-04-27
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 99.478(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.403(5)
_cell_length_b                   17.532(5)
_cell_length_c                   21.084(5)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     4887(3)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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 0.967
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48735
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         26.097
_diffrn_reflns_theta_min         2.046
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.99
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.50
_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
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.97
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1357
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         2942
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000212
_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: 
 4.73 -3.37 3.15 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1042
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2942
_reflns_number_total             2942
_reflns_threshold_expression     I>2.3\s(I)
_cod_data_source_file            ja9089389_si_004.cif
_cod_data_source_block           Compd_3
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C38 H55 Fe2 N18 O4.50 W1'
_cod_database_code               4102378