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_4321241
_publ_section_title
;
 Reactivity of Organometallic Molybdate toward Lanthanide Cations.
 Synthesis and Structure of Polynuclear Lanthanide-Molybdate Complexes
;
_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            'C32 H64 La3 Mo2 N7 O35'
_chemical_formula_weight         1715.51
_chemical_name_common            'dimeric La6Mo4'
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.44(2)
_cell_angle_beta                 115.41(2)
_cell_angle_gamma                86.45(2)
_cell_formula_units_Z            2
_cell_length_a                   12.661(3)
_cell_length_b                   22.168(3)
_cell_length_c                   11.691(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.43
_cell_measurement_theta_min      17.06
_cell_volume                     2953.5(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'RIGAKU AFC-5R'
_diffrn_measurement_method       \w-2\q
_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    0.1489
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26004
_diffrn_reflns_theta_full        35.10
_diffrn_reflns_theta_max         35.10
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        '-0.6, -5.5, -7.3'
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9097
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.567
_refine_diff_density_min         -3.197
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         26004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.2000
_reflns_number_gt                11631
_reflns_number_total             26004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991221c_2.cif
_cod_data_source_block           c:\shelx\sx97\yaglm1r
_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^)+(0.0900P)^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^)+(0.0900P)^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 
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_cod_original_cell_volume        2953.5(11)
_cod_database_code               4321241