Spin Equilibria in Monomeric Manganocenes: Solid-State Magnetic and EXAFS Studies
Walter, Marc D.; Sofield, Chadwick D.; Booth, Corwin H.; Andersen, Richard A.; Organometallics 28 (2009) 2005–; doi:10.1021/om800922j

data_4068541
_publ_section_title
;
 Spin Equilibria in Monomeric Manganocenes: Solid-State Magnetic and EXAFS
 Studies
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2005
_journal_paper_doi               10.1021/om800922j
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C34 H58 Mn'
_chemical_formula_sum            'C34 H58 Mn'
_chemical_formula_weight         521.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 112.483(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3262(4)
_cell_length_b                   17.6404(3)
_cell_length_c                   20.3767(4)
_cell_measurement_reflns_used    5533
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2
_cell_volume                     6418.9(3)
_computing_cell_refinement       'Bruker SAINT V. 6.40'
_computing_data_collection       'Bruker SMART V. 5.054D'
_computing_data_reduction        'Bruker SAINT V. 6.40'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      175(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       /w-scan
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27459
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.8892
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                6595
_reflns_number_total             10450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800922j_si_002.cif
_cod_data_source_block           tBu6Mn
_cod_original_cell_volume        6418.9(2)
_cod_original_sg_symbol_H-M      P2(1)/a
_cod_database_code               4068541