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_4115829
_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
'(py)8Yb4Se(Se2)4(SeC6H5)(SeC6H5)x(Se2C6H5)1-x + 2(py)'
_chemical_formula_sum            'C62 H60 N10 Se11.38 Yb4'
_chemical_formula_weight         2535.53
_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(6)
_cell_angle_beta                 92.25(4)
_cell_angle_gamma                90.00(5)
_cell_formula_units_Z            4
_cell_length_a                   12.405(6)
_cell_length_b                   30.97(2)
_cell_length_c                   18.881(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      16.9
_cell_measurement_theta_min      14.0
_cell_volume                     7248(7)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius CAD4 difractometer'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11137
_diffrn_reflns_theta_full        23.94
_diffrn_reflns_theta_max         23.94
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.869
_exptl_absorpt_correction_T_max  0.4636
_exptl_absorpt_correction_T_min  0.0655
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             4675
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.578
_refine_diff_density_min         -2.099
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.00002(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   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         11137
_refine_ls_number_restraints     1086
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1020P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                7812
_reflns_number_total             11137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011487u_3.cif
_cod_data_source_block           ybsean7
_cod_original_cell_volume        7249(7)
_cod_database_code               4115829