Synthesis of a series of 1,n'-disubstituted ferrocene derivatives containing disulfides
Shipmana, Patrick O; Lafrenierea, Matthew A; Colquhouna, Craig D S; Kraatz, Heinz-Bernhard; Inorganica Chimica Acta 391 (2012) 195–200; doi:10.1016/j.ica.2012.05.013

data_1508038
_publ_section_title
;
 Synthesis of a series of 1,n'-disubstituted ferrocene derivatives
 containing disulfides
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              195
_journal_page_last               200
_journal_paper_doi               10.1016/j.ica.2012.05.013
_journal_volume                  391
_journal_year                    2012
_chemical_formula_sum            'C20 H26 Fe N2 O5'
_chemical_formula_weight         430.28
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.698(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5371(10)
_cell_length_b                   5.7555(4)
_cell_length_c                   13.6054(10)
_cell_measurement_temperature    150(2)
_cell_volume                     970.44(13)
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0621
_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       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10954
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.8949
_exptl_absorpt_correction_T_min  0.8353
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.075(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4635
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                4019
_reflns_number_total             4635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-391-185-200.cif
_cod_data_source_block           09056
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1508038