Chalcogen-Rich Lanthanide Clusters with Fluorinated Thiolate Ligands
Mark Fitzgerald; Thomas J. Emge; John G. Brennan; Inorganic Chemistry 41 (2002) 3528–3532; doi:10.1021/ic020138d

data_4318170
_publ_contact_author_address
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  Department of Chemistry
  Rutgers, The State University of New Jersey
  610 Taylor Road
  Piscataway, New Jersey  08854-8087  U.S.A.
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_publ_contact_author_email       bren@rutchem.rutgers.edu
_publ_contact_author_name        'J. G. Brennan'
_publ_section_title
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 Chalcogen-Rich Lanthanide Clusters with Fluorinated Thiolate Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3528
_journal_page_last               3532
_journal_paper_doi               10.1021/ic020138d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C42 H60 F10 O7.5 S2 Se9 Yb4'
_chemical_formula_weight         2341.82
_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                63.60(4)
_cell_angle_beta                 87.42(4)
_cell_angle_gamma                89.94(4)
_cell_formula_units_Z            2
_cell_length_a                   12.082(8)
_cell_length_b                   16.018(5)
_cell_length_c                   17.528(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      17.9
_cell_measurement_theta_min      13.1
_cell_volume                     3035(3)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        local
_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 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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9412
_diffrn_reflns_theta_full        23.06
_diffrn_reflns_theta_max         23.06
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.648
_exptl_absorpt_correction_T_max  0.4106
_exptl_absorpt_correction_T_min  0.1989
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.712
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.00018(5)
_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   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         8394
_refine_ls_number_restraints     518
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0700P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                6998
_reflns_number_total             8394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020138d_2.cif
_cod_data_source_block           mark1red
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C42 H60 F10 O7.50 S2 Se9 Yb4'
_cod_database_code               4318170