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_4318169
_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 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            'C38.5 H53 F10 O6.63 S11 Yb4'
_chemical_formula_weight         1856.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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(2)
_cell_angle_beta                 91.52(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   12.252(2)
_cell_length_b                   17.763(6)
_cell_length_c                   27.199(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      17.9
_cell_measurement_theta_min      14.2
_cell_volume                     5917(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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10730
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.723
_exptl_absorpt_correction_T_max  0.7917
_exptl_absorpt_correction_T_min  0.3467
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3532
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.201
_refine_diff_density_min         -2.744
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9810
_refine_ls_number_restraints     1104
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1470
_reflns_number_gt                7254
_reflns_number_total             9810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020138d_1.cif
_cod_data_source_block           yb4s9scf2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        'C38.50 H53 F10 O6.63 S11 Yb4'
_cod_database_code               4318169