Preparation, characterization and electrochemical and X-ray structural studies of new conjugated 1,1'-ferrocenediyl-ended [CpFe-arylhydrazone]+ salts
Carolina Manzur; César Zúñiga; Lorena Millán; Mauricio Fuentealba; Jose A. Mata; Jean-René Hamon; David Carrillo; New J. Chem. 28 (2004) 134–144; doi:10.1039/b308626g

data_7050179
_publ_section_title
;
 Preparation, characterization and electrochemical and X-ray structural
 studies of new conjugated 1,1'-ferrocenediyl-ended
 [CpFe-arylhydrazone]+ salts
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              134
_journal_page_last               144
_journal_paper_doi               10.1039/b308626g
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C18 H18 F6 Fe1.5 N2 O P'
_chemical_formula_weight         507.09
_chemical_name_common
;
(1,1'-ferrocenedicarboxaldehyde-di((eta$5!-cyclopentadienyl)
(eta$6!-4-methoxiphenylhydrazone)iron(ii)))hexaflurophosphate
;
_chemical_name_systematic
;
{1,1'-ferrocenedicarboxaldehyde-di[(\h^5^-cyclopentadienyl)
(\h^6^-4-methoxiphenylhydrazone)iron(II)]}hexaflurophosphate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5730(11)
_cell_length_b                   16.5448(14)
_cell_length_c                   19.0521(16)
_cell_measurement_temperature    293(2)
_cell_volume                     3963.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0944
_diffrn_reflns_av_sigmaI/netI    0.2081
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27421
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_preparation       'Dichloromethane/Diethylether 1/1'
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00000(8)
_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   0.606
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.606
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          15.000
_refine_ls_shift/su_mean         0.057
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                1292
_reflns_number_total             4559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308626g.txt
_cod_data_source_block           mjdiome
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C18 H18 F6 Fe1.50 N2 O P'
_cod_database_code               7050179