Open-Shell Lanthanide(II+) or -(III+) Complexes Bearing σ-Silyl and Silylene Ligands: Synthesis, Structure, and Bonding Analysis.
Zitz, Rainer; Arp, Henning; Hlina, Johann; Walewska, Małgorzata; Marschner, Christoph; Szilvási, Tibor; Blom, Burgert; Baumgartner, Judith; Inorganic chemistry 54 (2015) 3306–3315; doi:10.1021/ic502991p

data_4342667
_publ_section_title
;
 Open-Shell Lanthanide(II+) or -(III+) Complexes Bearing \s-Silyl and
 Silylene Ligands: Synthesis, Structure, and Bonding Analysis.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3306
_journal_page_last               3315
_journal_paper_doi               10.1021/ic502991p
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C55 H111 K2 O12 Si8 Tm'
_chemical_formula_weight         1436.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 93.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.490(4)
_cell_length_b                   17.847(4)
_cell_length_c                   26.047(5)
_cell_measurement_reflns_used    29422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.472
_cell_measurement_theta_min      4.423
_cell_volume                     8118(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       '\w 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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62265
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         16507
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+22.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                14005
_reflns_number_total             16507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502991p_si_001.cif
_cod_data_source_block           2a_856j
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 4342667--4342674.cif.
;
_cod_original_cell_volume        8119(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4342667