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_4322790
_publ_contact_author             'John G. Brennan'
_publ_section_title
;
 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         'Sm(SeC6H5)3(NC5H5)3. 0.5(NC5H5)'
_chemical_formula_sum            'C35.5 H32.5 N3.5 Se3 Sm'
_chemical_formula_weight         895.38
_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                69.55(2)
_cell_angle_beta                 80.12(3)
_cell_angle_gamma                68.47(3)
_cell_formula_units_Z            2
_cell_length_a                   10.494(6)
_cell_length_b                   12.863(4)
_cell_length_c                   14.584(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(5)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      16.2
_cell_volume                     1713.7(13)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5992
_diffrn_reflns_theta_full        23.99
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.928
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   'numerical, Gaussian grid (SHELX76)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.06P)^2^+5.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0998
_refine_ls_wR_factor_ref         0.1032
_reflns_number_observed          4490
_reflns_number_total             5261
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9716161_5.cif
_cod_data_source_block           pyrsmse
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.06P)^2^+5.0P] 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^)+(0.06P)^2^+5.0P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1713.7(12)
_cod_original_formula_sum        'C35.50 H32.50 N3.50 Se3 Sm'
_cod_database_code               4322790