Fluorinated Thiolates of Divalent and Trivalent Lanthanides. Ln-F Bonds and the Synthesis of LnF3
Jonathan H. Melman; Thomas J. Emge; John G. Brennan; Inorganic Chemistry 40 (2001) 1078–1081; doi:10.1021/ic0006908

data_4319297
_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
;
 Fluorinated Thiolates of Divalent and Trivalent Lanthanides. Ln-F Bonds
 and the Synthesis of LnF3
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1078
_journal_page_last               1081
_journal_paper_doi               10.1021/ic0006908
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[(C4H8O)2Sm(SC6F5)3]2'
_chemical_formula_sum            'C26 H16 F15 O2 S3 Sm'
_chemical_formula_weight         891.92
_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                 92.27(7)
_cell_angle_gamma                90.00(6)
_cell_formula_units_Z            4
_cell_length_a                   11.923(10)
_cell_length_b                   12.404(7)
_cell_length_c                   19.869(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      10.0
_cell_volume                     2936(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.1429
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5101
_diffrn_reflns_theta_full        23.98
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.335
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_correction_T_min  0.8058
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.276
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     687
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1670
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                2428
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006908_2.cif
_cod_data_source_block           smsc6f5
_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 
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_cod_database_code               4319297