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_4065169
_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, 3(C3 H6 O), 2(F6 P)'
_chemical_formula_sum            'C45 H50 F12 Fe2 N2 O3 P2'
_chemical_formula_weight         1068.51
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.318(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.310(4)
_cell_length_b                   9.5057(7)
_cell_length_c                   17.0926(10)
_cell_measurement_reflns_used    4364
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3686
_cell_measurement_theta_min      2.6994
_cell_volume                     4647.4(8)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 2'
_diffrn_measurement_method       'omega and phi 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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11078
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70499
_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    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0610P)^2^+44.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.2097
_reflns_number_gt                2516
_reflns_number_total             4031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200604f_si_002.cif
_cod_data_source_block           '[5][PF6]2.3Me2CO'
_cod_original_cell_volume        4647.5(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4065169