Trivalent Lanthanide Compounds with Fluorinated Thiolate Ligands: Ln-F Dative Interactions Vary with Ln and Solvent
Jonathan H. Melman; Christa Rohde; Thomas J. Emge; John G. Brennan; Inorganic Chemistry 41 (2002) 28–33; doi:10.1021/ic0104813

data_4317380
_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
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 Trivalent Lanthanide Compounds with Fluorinated Thiolate Ligands: Ln-F
 Dative Interactions Vary with Ln and Solvent
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              28
_journal_page_last               33
_journal_paper_doi               10.1021/ic0104813
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H24 Ce F15 O3 S3'
_chemical_formula_weight         953.79
_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                71.77(3)
_cell_angle_beta                 76.36(4)
_cell_angle_gamma                84.90(3)
_cell_formula_units_Z            2
_cell_length_a                   11.055(5)
_cell_length_b                   12.377(5)
_cell_length_c                   13.216(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      12.5
_cell_volume                     1668.9(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5648
_diffrn_reflns_theta_full        24.19
_diffrn_reflns_theta_max         24.19
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.669
_exptl_absorpt_correction_T_max  0.7544
_exptl_absorpt_correction_T_min  0.6258
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         5334
_refine_ls_number_restraints     849
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0400P)^2^+3.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4831
_reflns_number_total             5334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104813_2.cif
_cod_data_source_block           cescfthf
_cod_depositor_comments
;
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_database_code               4317380