Heterometallic Chalcogenido Clusters Containing Lanthanides and Main Group Metals: Emissive Precursors to Ternary Solid-State Compounds
Anna Kornienko; Santanu Banerjee; G. Ajith Kumar; Richard E. Riman; Thomas J. Emge; John G. Brennan; Journal of the American Chemical Society 127 (2005) 14008–14014; doi:10.1021/ja0534708

data_4111960
_publ_section_title
;
 Heterometallic Chalcogenido Clusters Containing Lanthanides and Main
 Group Metals: Emissive Precursors to Ternary Solid-State Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14008
_journal_page_last               14014
_journal_paper_doi               10.1021/ja0534708
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C64 H60 Hg2 N8 Se10.08 Yb4'
_chemical_formula_weight         2830.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 111.849(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9070(6)
_cell_length_b                   17.5001(8)
_cell_length_c                   16.9594(8)
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.33
_cell_volume                     3555.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD diffractometer'
_diffrn_measurement_method       'omege and phi 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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35967
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.713
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.644
_exptl_crystal_description       needle
_exptl_crystal_F_000             2565
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.553
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.248
_refine_ls_extinction_coef       0.00003(3)
_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   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         8822
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                6548
_reflns_number_total             8822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0534708si20050526_052750.cif
_cod_data_source_block           yb4hg2se6m
_cod_database_code               4111960