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_4317382
_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
;
 Trivalent Lanthanide Compounds with Fluorinated Thiolate Ligands: Ln-F
 Dative Interactions Vary with Ln and Solvent
;
_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            'C40.5 H22.5 F15 N4.5 S3 Sm'
_chemical_formula_weight         1103.66
_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                108.96(4)
_cell_angle_beta                 92.21(3)
_cell_angle_gamma                95.00(3)
_cell_formula_units_Z            2
_cell_length_a                   9.510(3)
_cell_length_b                   14.644(5)
_cell_length_c                   15.911(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      11.1
_cell_volume                     2082.4(16)
_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 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Nonius CAD4 difractometer'
_diffrn_measurement_method       '\q-\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6005
_diffrn_reflns_theta_full        23.23
_diffrn_reflns_theta_max         23.23
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.7583
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELX-76
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     978
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                3686
_reflns_number_total             5568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104813_4.cif
_cod_data_source_block           sm2fsp
_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_original_cell_volume        2082.4(15)
_cod_original_formula_sum        'C40.50 H22.50 F15 N4.50 S3 Sm'
_cod_database_code               4317382