Synthesis and Structural Studies of 1,1'-Bis-Amino-Functionalized Ferrocenes, Ferrocene Salts, and Ferrocenium Salts
Sam Bradley; Kenneth D. Camm; Xiaoming Liu; Patrick C. McGowan; Raheela Mumtaz; Karrie A. Oughton; Thomas J. Podesta; Mark Thornton-Pett; Inorganic Chemistry 41 (2002) 715–726; doi:10.1021/ic010821k

data_4317563
_publ_contact_author
;
     Patrick McGowan
     School of Chemistry
     University of Leeds
     Leeds LS2 9JT
     UK
;
_publ_contact_author_email       patrickm@chem.leeds.ac.uk
_publ_contact_author_fax         '+44 (0)113 2336565'
_publ_contact_author_phone       '+44 (0)113 2336404'
_publ_section_title
;
 Synthesis and Structural Studies of 1,1'-Bis-Amino-Functionalized
 Ferrocenes, Ferrocene Salts, and Ferrocenium Salts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              715
_journal_page_last               726
_journal_paper_doi               10.1021/ic010821k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H38 B2 F8 Fe N2'
_chemical_formula_weight         584.03
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.4780(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4954(2)
_cell_length_b                   6.16440(10)
_cell_length_c                   31.6684(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2626.49(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            21359
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.9561
_exptl_absorpt_correction_T_min  0.7011
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          1.171
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+1.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                3725
_reflns_number_total             5167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010821k_6.cif
_cod_data_source_block           kcx4y
_cod_original_cell_volume        2626.48(8)
_cod_database_code               4317563