Chalcogen-Rich Lanthanide Clusters: Cluster Reactivity and the Influence of Ancillary Ligands on Structure
Anna Y. Kornienko; Thomas J. Emge; John G. Brennan; Journal of the American Chemical Society 123 (2001) 11933–11939; doi:10.1021/ja011487u

data_4115828
_publ_contact_author_address
; 
 Department of Chemistry 
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey  08854-8087  U.S.A. 
;
_publ_contact_author_email       bren@rutchem.rutgers.edu
_publ_contact_author_name        'J. G. Brennan'
_publ_section_title
;
 Chalcogen-Rich Lanthanide Clusters: Cluster Reactivity and the Influence
 of Ancillary Ligands on Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11933
_journal_page_last               11939
_journal_paper_doi               10.1021/ja011487u
_journal_volume                  123
_journal_year                    2001
_chemical_formula_moiety         '(NC5H5)8Yb4Se6(SC6H5)4 + 2(NC5H5)'
_chemical_formula_sum            'C37 H35 N5 S2 Se3 Yb2'
_chemical_formula_weight         1196.78
_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                91.27(5)
_cell_angle_beta                 89.89(5)
_cell_angle_gamma                110.14(6)
_cell_formula_units_Z            2
_cell_length_a                   10.928(9)
_cell_length_b                   12.960(9)
_cell_length_c                   14.658(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      11.9
_cell_volume                     1949(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6476
_diffrn_reflns_theta_full        24.03
_diffrn_reflns_theta_max         24.03
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.712
_exptl_absorpt_correction_T_max  0.4798
_exptl_absorpt_correction_T_min  0.3754
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_description       lathe
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.00045(11)
_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   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6108
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4825
_reflns_number_total             6108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011487u_2.cif
_cod_data_source_block           yb4se6sp
_cod_database_code               4115828