Trivalent Lanthanide Chalcogenolates: Ln(SePh)3, Ln2(EPh)6, Ln4(SPh)12, and [Ln (EPh)3]n(E = S, Se). How Metal, Chalcogen, and Solvent Influence Structure
Jongseong Lee; Deborah Freedman; Jonathan H. Melman; Meggan Brewer; Lei Sun; T. J. Emge; F. H. Long; John G. Brennan; Inorganic Chemistry 37 (1998) 2512–2519; doi:10.1021/ic9716161

data_4322788
_publ_contact_author             'John G. Brennan'
_publ_section_title
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 Trivalent Lanthanide Chalcogenolates: Ln(SePh)3, Ln2(EPh)6, Ln4(SPh)12,
 and [Ln (EPh)3]n(E = S, Se). How Metal, Chalcogen, and Solvent Influence
 Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2512
_journal_page_last               2519
_journal_paper_doi               10.1021/ic9716161
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'Sm2(SC6H5)6(NC5H5)4. (OC4H10)'
_chemical_formula_sum            'C60 H60 N4 O S6 Sm2'
_chemical_formula_weight         1346.18
_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(2)
_cell_angle_beta                 102.37(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   13.488(3)
_cell_length_b                   31.085(3)
_cell_length_c                   14.429(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      9.0
_cell_volume                     5909.3(19)
_computing_cell_refinement       'CAD4 (Enraf Nonius)'
_computing_data_collection       'CAD4 (Enraf Nonius)'
_computing_data_reduction        'CAD4 (Enraf Nonius)'
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CAD4 diffractometer'
_diffrn_measurement_method       'omega 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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7260
_diffrn_reflns_theta_full        21.48
_diffrn_reflns_theta_max         21.48
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.222
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   'numerical, Gaussian grid (SHELX76)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     1012
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_obs          0.0557
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.055P)^2^+5.5P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1195
_refine_ls_wR_factor_ref         0.1309
_reflns_number_observed          4450
_reflns_number_total             6739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9716161_3.cif
_cod_data_source_block           sms3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.055P)^2^+5.5P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.055P)^2^+5.5P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322788