Stabilization of molecular lanthanide polysulfides by bulky scorpionate ligands.
Kühling, Marcel; McDonald, Robert; Liebing, Phil; Hilfert, Liane; Ferguson, Michael J.; Takats, Josef; Edelmann, Frank T.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10118–10121; doi:10.1039/c6dt01439a

data_7039139
_publ_section_title
;
 Stabilization of molecular lanthanide polysulfides by bulky scorpionate
 ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10118
_journal_page_last               10121
_journal_paper_doi               10.1039/c6dt01439a
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C90 H154 B2 N20 S4 Yb2, 2(C5 H12)'
_chemical_formula_sum            'C100 H178 B2 N20 S4 Yb2'
_chemical_formula_weight         2156.55
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1lfl1n
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-07 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.597(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.7535(5)
_cell_length_b                   17.0849(5)
_cell_length_c                   16.4796(4)
_cell_measurement_reflns_used    19624
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.138
_cell_measurement_theta_min      1.954
_cell_volume                     5654.6(3)
_computing_cell_refinement       'X-Area (STOE & Cie, 1999)'
_computing_data_collection       'X-Area (STOE & Cie, 1999)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 1999)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19624
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.138
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_T_max  0.8078
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area and X-Red (STOE & Cie, 1999)'
_exptl_crystal_colour            rose
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       rod
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.991
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11252
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0352
_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^)+(0.1169P)^2^+4.2180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10767
_reflns_number_total             11252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01439a2.cif
_cod_data_source_block           li0003
_cod_depositor_comments
'Adding full bibliography for 7039139--7039141.cif.'
_cod_database_code               7039139
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.843
_shelx_res_checksum              44785