57Fe-Labeled Octamethylferrocenium Tetrafluoroborate. X-ray Crystal Structures of Conformational Isomers, Hyperfine Interactions, and Spin-Lattice Relaxation by Moessbauer Spectroscopy
Herwig Schottenberger; Klaus Wurst; Ulrich J. Griesser; Ram K. R. Jetti; Gerhard Laus; Rolfe H. Herber; Israel Nowik; Journal of the American Chemical Society 127 (2005) 6795–6801; doi:10.1021/ja050452h

data_4111689
_publ_section_title
;
 57Fe-Labeled Octamethylferrocenium Tetrafluoroborate. X-ray Crystal
 Structures of Conformational Isomers, Hyperfine Interactions, and
 Spin-Lattice Relaxation by Moessbauer Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6795
_journal_page_last               6801
_journal_paper_doi               10.1021/ja050452h
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C18 H26 B F4 Fe'
_chemical_formula_weight         385.05
_chemical_name_systematic
; 
 ? 
;
_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                 94.353(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4000(10)
_cell_length_b                   8.5030(10)
_cell_length_c                   25.916(4)
_cell_measurement_reflns_used    23047
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      1.0
_cell_volume                     1845.7(4)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'phi- and omega-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  0.1039
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6301
_diffrn_reflns_theta_full        20.49
_diffrn_reflns_theta_max         20.49
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         1855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                1186
_reflns_number_total             1855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050452hsi20050123_105337_2.cif
_cod_data_source_block           CCDC249286
_cod_database_code               4111689