Synthesis, Crystal and Electronic Structures, and Physical Properties of the Novel Compounds LaR4Mo36O52 (R = Dy, Er, Yb, and Y) Containing Infinite Chains of Trans-Edge-Shared Mo6 Octahedra and Mo2 Pairs and Rectangular Mo4 Clusters with Triple Mo-Mo Bonds
N. Barrier; B. Fontaine; S. Pierrefixe; R. Gautier; P. Gougeon; Inorganic Chemistry 48 (2009) 3848–3856; doi:10.1021/ic801942d

data_4301932
_publ_section_title
;
Synthesis, Crystal and Electronic Structures, and Physical Properties of
the Novel Compounds LaR4Mo36O52 (R = Dy, Er, Yb, and Y) Containing Infinite
Chains of Trans-Edge-Shared Mo6 Octahedra and Mo2 Pairs and Rectangular
Mo4 Clusters with Triple Mo-Mo Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3848
_journal_page_last               3856
_journal_paper_doi               10.1021/ic801942d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Er4 La Mo36 O52'
_chemical_formula_weight         5093.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   19.8348(2)
_cell_length_b                   19.8348(2)
_cell_length_c                   5.65940(10)
_cell_measurement_reflns_used    30231
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.78
_cell_measurement_theta_min      1.00
_cell_volume                     2226.52(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35107
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    18.225
_exptl_absorpt_correction_T_max  0.1388
_exptl_absorpt_correction_T_min  0.0511
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'black needles with square cross section'
_exptl_crystal_F_000             4514
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.019
_refine_diff_density_max         3.955
_refine_diff_density_min         -2.732
_refine_diff_density_rms         0.471
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.507(12)
_refine_ls_extinction_coef       0.00032(2)
_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   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+64.3224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                5576
_reflns_number_total             5922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801942d_si_001.cif
_cod_data_source_block           la
_cod_database_code               4301932