Reactivity of Organometallic Molybdate toward Lanthanide Cations. Synthesis and Structure of Polynuclear Lanthanide-Molybdate Complexes
M. Hashimoto; M. Takata; A. Yagasaki; Inorganic Chemistry 39 (2000) 3712–3714; doi:10.1021/ic991221c

data_4321242
_publ_section_title
;
 Reactivity of Organometallic Molybdate toward Lanthanide Cations.
 Synthesis and Structure of Polynuclear Lanthanide-Molybdate Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3712
_journal_page_last               3714
_journal_paper_doi               10.1021/ic991221c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C28 H66 Ce3 Mo2 N7 O38'
_chemical_formula_weight         1721.12
_chemical_name_common            (Ce6Mo4)(Ce3Mo2)2_ion_pair
_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                97.65(4)
_cell_angle_beta                 102.75(3)
_cell_angle_gamma                102.52(4)
_cell_formula_units_Z            4
_cell_length_a                   21.387(6)
_cell_length_b                   30.37(2)
_cell_length_c                   12.441(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.12
_cell_measurement_theta_min      15.40
_cell_volume                     7554(7)
_computing_cell_refinement       TEXSAN
_computing_data_collection       TEXSAN
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    ORTEPII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'RIGAKU AFC-5R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2875
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26589
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        -12.5,1.8,-4.8
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7915
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.955
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.00036(9)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         26589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.2693
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2346
_refine_ls_wR_factor_ref         0.3050
_reflns_number_gt                9874
_reflns_number_total             26589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991221c_3.cif
_cod_data_source_block           yagcm1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+0.0000P] 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^)+(0.1300P)^2^+0.0000P] 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        7554(6)
_cod_database_code               4321242