Slow Magnetic Relaxation in Trigonal-Planar Mononuclear Fe(II) and Co(II) Bis(trimethylsilyl)amido Complexes-A Comparative Study.
Eichhöfer, Andreas; Lan, Yanhua; Mereacre, Valeriu; Bodenstein, Tilmann; Weigend, Florian; Inorganic chemistry 53 (2014) 1962–1974; doi:10.1021/ic401677j

data_4337249
_publ_section_title
;
 Slow Magnetic Relaxation in Trigonal-Planar Mononuclear Fe(II) and Co(II)
 Bis(trimethylsilyl)amido Complexes-A Comparative Study.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1962
_journal_page_last               1974
_journal_paper_doi               10.1021/ic401677j
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '[Li15-crown-5][Fe(N(Si(CH3)3)2)3]'
_chemical_formula_sum            'C29 H76 Cl2 Fe Li N3 O5 Si6'
_chemical_formula_weight         849.16
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.614(3)
_cell_length_b                   20.523(4)
_cell_length_c                   16.710(3)
_cell_measurement_reflns_used    19866
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.22
_cell_volume                     4772.6(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND2.1 (Brandenburger, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22197
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale beige'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       elongated
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+2.6877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                6878
_reflns_number_total             8890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401677j_si_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        4772.4(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4337249