A pillared discrete bilayer formed from guanidinium and ferrocenedisulfonate ions: synthesis, crystal structure, and initial electrochemical properties.
Xie, Jingli; Ma, Michelle T.; Abrahams, Brendan F.; Wedd, Anthony G.; Inorganic chemistry 46 (2007) 9027–9029; doi:10.1021/ic7011974

data_4339030
_publ_section_title
;
 A pillared discrete bilayer formed from guanidinium and
 ferrocenedisulfonate ions: synthesis, crystal structure, and initial
 electrochemical properties.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9027
_journal_page_last               9029
_journal_paper_doi               10.1021/ic7011974
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C12 H20 Fe N6 O6 S2'
_chemical_formula_weight         464.31
_chemical_name_systematic
; 
 ? 
;
_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                98.283(10)
_cell_angle_beta                 100.122(9)
_cell_angle_gamma                118.767(7)
_cell_formula_units_Z            1
_cell_length_a                   7.269(4)
_cell_length_b                   7.307(4)
_cell_length_c                   11.469(5)
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      6
_cell_volume                     506.9(5)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.692
_diffrn_measured_fraction_theta_max 0.692
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.1176
_diffrn_reflns_av_sigmaI/netI    0.3517
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1483
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.000(18)
_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   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1238
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.3909
_refine_ls_R_factor_gt           0.2832
_refine_ls_shift/su_max          1.019
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.3500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5609
_refine_ls_wR_factor_ref         0.6197
_reflns_number_gt                367
_reflns_number_total             1238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011974-file002.cif
_cod_data_source_block           jl81221m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        506.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339030