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_4322731
_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     '[Cr(OH)6Mo6O18] [Fe(C5(CH3)5)2]3 20H2O'
_chemical_formula_sum            'C60 H136 Cr Fe3 Mo6 O44'
_chemical_formula_weight         2356.88
_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
_cell_angle_alpha                101.55(2)
_cell_angle_beta                 105.82(2)
_cell_angle_gamma                110.23(2)
_cell_formula_units_Z            1
_cell_length_a                   12.489(3)
_cell_length_b                   14.113(3)
_cell_length_c                   15.662(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.42
_cell_measurement_theta_min      4.46
_cell_volume                     2355.8(12)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9777
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        +2.9
_diffrn_standards_interval_count 250
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.8102
_exptl_absorpt_correction_type   'Semi empirical \y-scan'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       'Green octaedron'
_exptl_crystal_F_000             1202
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0109(4)
_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_all   1.001
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      1.041
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+5.0958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1223
_refine_ls_wR_factor_obs         0.0968
_reflns_number_observed          5598
_reflns_number_total             9298
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971221h_2.cif
_cod_data_source_block           fecr(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+5.0958P] 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^)+(0.0532P)^2^+5.0958P] 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        2355.7(9)
_cod_database_code               4322731