Chalcogen-Rich Lanthanide Clusters: Compounds with Te2-, (TeTe)2-, TePh, TeTePh, (TeTeTe(Ph)TeTe)5-, and [(TeTe)4TePh]9- Ligands; Single Source Precursors to Solid-State Lanthanide Tellurides
Deborah Freedman; Thomas J. Emge; John G. Brennan; Inorganic Chemistry 41 (2002) 492–500; doi:10.1021/ic010981w

data_4317516
_publ_section_title
;
 Chalcogen-Rich Lanthanide Clusters: Compounds with Te2-, (TeTe)2-, TePh,
 TeTePh, (TeTeTe(Ph)TeTe)5-, and [(TeTe)4TePh]9- Ligands; Single Source
 Precursors to Solid-State Lanthanide Tellurides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              492
_journal_page_last               500
_journal_paper_doi               10.1021/ic010981w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C62 H60 N10 Te11.57 Tm4'
_chemical_formula_weight         3097.25
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(6)
_cell_angle_beta                 113.38(4)
_cell_angle_gamma                90.00(4)
_cell_formula_units_Z            4
_cell_length_a                   23.407(7)
_cell_length_b                   23.20(2)
_cell_length_c                   17.507(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      13.0
_cell_volume                     8726(10)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'local program'
_computing_molecular_graphics    'XPMA/ZORTEP (Zsolnai, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(5)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius CAD4 diffractometer'
_diffrn_measurement_method       '\w-\q scans'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6751
_diffrn_reflns_theta_full        23.45
_diffrn_reflns_theta_max         23.45
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.855
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5519
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.418
_refine_diff_density_min         -3.191
_refine_diff_density_rms         0.380
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         6556
_refine_ls_number_restraints     821
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1500P)^2^+250.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2403
_reflns_number_gt                4109
_reflns_number_total             6556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010981w_3.cif
_cod_data_source_block           tm4s2
_cod_original_cell_volume        8728(9)
_cod_database_code               4317516