Slow Magnetic Relaxation in a Family of trigonal Pyramidal Iron(II) Pyrrolide Complexes
W. Hill Harman; T. David Harris; Danna E. Freedman; Henry Fong; Alicia Chang; Jeffrey D. Rinehart; Andrew Ozarowski; Moulay T. Sougrati; Fernande Grandjean; Gary J. Long; Jeffrey R. Long; Christopher J. Chang; Journal of the American Chemical Society 132 (2010) 18115–18126; doi:10.1021/ja105291x

data_4103709
_publ_section_title
;
 Slow Magnetic Relaxation in a Family of trigonal Pyramidal Iron(II)
 Pyrrolide Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18115
_journal_page_last               18126
_journal_paper_doi               10.1021/ja105291x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C12 H30 Na O6, C33 H27 Fe N4'
_chemical_formula_sum            'C45 H57 Fe N4 Na O6'
_chemical_formula_weight         828.79
_chemical_name_common            '[Na(DME)3][tpaPhFe]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.897(2)
_cell_angle_beta                 73.871(2)
_cell_angle_gamma                69.850(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3600(17)
_cell_length_b                   12.0280(18)
_cell_length_c                   17.881(3)
_cell_measurement_reflns_used    4798
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2180.0(6)
_computing_cell_refinement       'Bruker APEX2 v. 2009.3'
_computing_data_collection       'Bruker APEX2 v. 2009.3'
_computing_data_reduction        'Bruker APEX2 v. 2009.3'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  ORTEP-32
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16928
_diffrn_reflns_theta_full        25.76
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+1.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                5411
_reflns_number_total             8139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105291x_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4103709