Preparation, Crystal Structures, and Magnetic and ESR Properties of Molecular Assemblies of Ferrocenium Derivatives and Paramagnetic Polyoxometalates
Stéphane Golhen; Lahcène Ouahab; Daniel Grandjean; Philippe Molinié; Inorganic Chemistry 37 (1998) 1499–1506; doi:10.1021/ic971221h

data_4322733
_publ_section_title
;
 Preparation, Crystal Structures, and Magnetic and ESR Properties of
 Molecular Assemblies of Ferrocenium Derivatives and Paramagnetic
 Polyoxometalates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1499
_journal_page_last               1506
_journal_paper_doi               10.1021/ic971221h
_journal_volume                  37
_journal_year                    1998
_chemical_formula_structural     '[Fe(C5(CH3)5)2]4 HPCu(H2O)W11O39 6(CH3CN)'
_chemical_formula_sum            'C92 H141 Cu Fe4 N6 O40 P W11'
_chemical_formula_weight         4311.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.596(7)
_cell_length_b                   15.138(3)
_cell_length_c                   25.921(12)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    287(2)
_cell_measurement_theta_max      12.041
_cell_measurement_theta_min      7.071
_cell_volume                     6067(4)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        MolEN
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      287(2)
_diffrn_measurement_device       'Enraf Nonius 4-circle diffractometer'
_diffrn_measurement_method       \q-2\q
_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  0.1406
_diffrn_reflns_av_sigmaI/netI    0.3363
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13681
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        14.3
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.099
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_correction_T_min  0.4715
_exptl_absorpt_correction_type   'semi-empirical \y-scan'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.360
_exptl_crystal_description       'Green octahedron block'
_exptl_crystal_F_000             4034
_refine_diff_density_max         1.891
_refine_diff_density_min         -3.519
_refine_diff_density_rms         0.455
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.302
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         13153
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_restrained_S_obs      1.305
_refine_ls_R_factor_all          0.3170
_refine_ls_R_factor_obs          0.0817
_refine_ls_shift/esd_max         -4.117
_refine_ls_shift/esd_mean        0.349
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+291.7159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2618
_refine_ls_wR_factor_obs         0.1787
_reflns_number_observed          4487
_reflns_number_total             13161
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971221h_4.cif
_cod_data_source_block           fecu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+291.7159P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+291.7159P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6067.2(41)
_cod_database_code               4322733