A Surprising Solvent Effect on the Crystal Structure of an Anionic Lanthanide Sandwich Complex†
Lorenz, Volker; Edelmann, Anja; Blaurock, Steffen; Freise, Fritjof; Edelmann, Frank T.; Organometallics 26 (2007) 6681–; doi:10.1021/om7006776

data_4073850
_publ_section_title
;
 A Surprising Solvent Effect on the Crystal Structure of an Anionic
 Lanthanide Sandwich Complex&#x2020;
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6681
_journal_paper_doi               10.1021/om7006776
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C37 H70 Li O2 Si4 Tb'
_chemical_formula_weight         825.15
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_beta                 104.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.059(3)
_cell_length_b                   14.773(3)
_cell_length_c                   22.533(5)
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      2.03
_cell_volume                     4534.8(18)
_computing_cell_refinement       'Stoe XAREA'
_computing_data_collection       'Stoe XAREA'
_computing_data_reduction        'Stoe XAREA'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'Bruker SHELXTL PLUS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43029
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.5510
_exptl_absorpt_correction_T_min  0.4851
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         12162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.290
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                8723
_reflns_number_total             12162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7006776-file004.cif
_cod_data_source_block           ip2_196b
_cod_original_cell_volume        4535.0(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4073850