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_4317561
_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 H34 F6 Fe N2 O4'
_chemical_formula_weight         584.38
_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                 100.2990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   12.2379(2)
_cell_length_b                   31.2235(7)
_cell_length_c                   21.5825(5)
_cell_measurement_temperature    150(2)
_cell_volume                     8114.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38755
_diffrn_reflns_theta_full        23.52
_diffrn_reflns_theta_max         23.52
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.8842
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         9.081
_refine_diff_density_min         -1.839
_refine_diff_density_rms         0.492
_refine_ls_extinction_coef       0.035(10)
_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   6.702
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         11857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      6.702
_refine_ls_R_factor_all          0.6224
_refine_ls_R_factor_gt           0.5574
_refine_ls_shift/su_max          2.502
_refine_ls_shift/su_mean         1.299
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.8564
_refine_ls_wR_factor_ref         0.8831
_reflns_number_gt                6201
_reflns_number_total             11857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010821k_4.cif
_cod_data_source_block           rah1
_cod_database_code               4317561