Cymantrene Radical Cation Family: Spectral and Structural Characterization of the Half-Sandwich Analogues of Ferrocenium Ion
Derek R. Laws; Daesung Chong; Karen Nash; Arnold L. Rheingold; William E. Geiger; Journal of the American Chemical Society 130 (2008) 9859–9870; doi:10.1021/ja801930q

data_4108105
_publ_section_title
;
 Cymantrene Radical Cation Family: Spectral and Structural
 Characterization of the Half-Sandwich Analogues of Ferrocenium Ion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9859
_journal_page_last               9870
_journal_paper_doi               10.1021/ja801930q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C32 H14 B F20 Mn N O7'
_chemical_formula_weight         970.19
_chemical_name_systematic
; 

 ? 

;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 111.6160(10)
_cell_angle_gamma                102.7390(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1365(8)
_cell_length_b                   11.5717(8)
_cell_length_c                   14.7086(10)
_cell_measurement_reflns_used    5464
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.62
_cell_volume                     1636.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10223
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.8845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       plate
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                4924
_reflns_number_total             6206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801930q-file006.cif
_cod_data_source_block           geiger5
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