Ferrocenyl Diquat Derivatives: Nonlinear Optical Activity, Multiple Redox States, and Unusual Reactivity
Coe, Benjamin J.; Fielden, John; Foxon, Simon P.; Asselberghs, Inge; Clays, Koen; Van Cleuvenbergen, Stijn; Brunschwig, Bruce S.; Organometallics 30 (2011) 5731–; doi:10.1021/om200604f

data_4065170
_publ_section_title
;
 Ferrocenyl Diquat Derivatives: Nonlinear Optical Activity, Multiple Redox
 States, and Unusual Reactivity
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5731
_journal_paper_doi               10.1021/om200604f
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C36 H32 Fe2 N2, 2(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C42 H41 F12 Fe2 N5 P2'
_chemical_formula_weight         1017.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.48(1)
_cell_angle_beta                 84.16(1)
_cell_angle_gamma                70.41(1)
_cell_formula_units_Z            2
_cell_length_a                   10.011(1)
_cell_length_b                   14.438(2)
_cell_length_c                   16.104(2)
_cell_measurement_reflns_used    2748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4094
_cell_measurement_theta_min      2.6296
_cell_volume                     2102.3(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.741
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.2145
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10826
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         7893
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1895
_refine_ls_R_factor_gt           0.0969
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1498P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2860
_reflns_number_gt                3749
_reflns_number_total             7893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200604f_si_002.cif
_cod_data_source_block           '[5][PF6]2.3MeCN'
_cod_original_cell_volume        2102.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065170