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_4322786
_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         '{Nd3(SeC6H5)9(OC4H8)4. 2.125(OC4H8)}n'
_chemical_formula_sum            'C78.5 H94 Nd3 O6.125 Se9'
_chemical_formula_weight         2278.90
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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(9)
_cell_angle_beta                 128.93(2)
_cell_angle_gamma                90.00(8)
_cell_formula_units_Z            8
_cell_length_a                   34.232(9)
_cell_length_b                   25.526(11)
_cell_length_c                   27.358(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(7)
_cell_measurement_theta_max      15.6
_cell_measurement_theta_min      13.2
_cell_volume                     18596(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      203(7)
_diffrn_measured_fraction_theta_full 0.495
_diffrn_measured_fraction_theta_max 0.495
_diffrn_measurement_device_type  'CAD4 diffractometer'
_diffrn_measurement_method       'omega:theta 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  0.1150
_diffrn_reflns_av_sigmaI/netI    0.1630
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13524
_diffrn_reflns_theta_full        18.03
_diffrn_reflns_theta_max         18.03
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.216
_exptl_absorpt_correction_T_max  0.8496
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   'numerical, Gaussian grid (SHELX76)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             8800
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.651
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         6378
_refine_ls_number_restraints     1785
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_obs          0.0728
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.09P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1632
_refine_ls_wR_factor_ref         0.1863
_reflns_number_observed          3328
_reflns_number_total             6378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9716161_1.cif
_cod_data_source_block           ndsethf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.09P)^2^] 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^)+(0.09P)^2^] 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        18596(12)
_cod_database_code               4322786