The first observation of the [Cp3Mn]– anion; structures of hexagonal [(η2-Cp)3MnK·1.5thf] and ion-separated [(η2-Cp)3Mn]2[Mg(thf)6]·2thf
Bond, Andrew D.; Layfield, Richard A.; MacAllister, Judith A.; Rawson, Jeremy M.; Wright, Dominic S.; McPartlin, Mary; Chemical Communications  (2001) 1956–; doi:10.1039/b106366a

data_7115028
_publ_section_title
;
 The first observation of the [Cp3Mn]-- anion; structures of hexagonal
 [(\h2-Cp)3MnK&#x00B7;1.5thf] and ion-separated
 [(\h2-Cp)3Mn]2[Mg(thf)6]&#x00B7;2thf
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1956
_journal_paper_doi               10.1039/b106366a
_journal_year                    2001
_chemical_formula_moiety         '(Mn (C5 H5)3)2, Mg (C4 H8 O)6, (C4 H8 O)2'
_chemical_formula_sum            'C62 H94 Mg Mn2 O8'
_chemical_formula_weight         1101.56
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.560(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0027(9)
_cell_length_b                   10.7118(6)
_cell_length_c                   24.0194(10)
_cell_measurement_reflns_used    12535
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     5940.7(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.860
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f 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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18733
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  1.071
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+17.8103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                3374
_reflns_number_total             4500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106366a.txt
_cod_data_source_block           dw0117
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115028