Synthesis and First Structural Characterization of Lanthanide(II) Aryls: Observation of a Schlenk Equilibrium in Europium(II) and Ytterbium(II) Chemistry
Gernot Heckmann; Mark Niemeyer; Journal of the American Chemical Society 122 (2000) 4227–4228; doi:10.1021/ja993494c

data_4115989
_publ_contact_author_address
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Institut f\"ur Anorganische Chemie
Universit\"at Stuttgart
Pfaffenwaldring 55
D-70569 Stuttgart
Germany
;
_publ_contact_author_email       niemeyer@iac.uni-stuttgart.de
_publ_contact_author_name        'Mark Niemeyer'
_publ_section_title
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 Synthesis and First Structural Characterization of Lanthanide(II) Aryls:
 Observation of a Schlenk Equilibrium in Europium(II) and Ytterbium(II)
 Chemistry
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4227
_journal_page_last               4228
_journal_paper_doi               10.1021/ja993494c
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C80 H160 Eu4 I8 O20'
_chemical_formula_weight         3065.12
_chemical_melting_point          546
_chemical_name_systematic
; 
Pentakis(tetrahydofuran)diiodoeuropium(II) 
;
_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                 111.093(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.163(6)
_cell_length_b                   26.096(5)
_cell_length_c                   23.981(6)
_cell_measurement_temperature    173(2)
_cell_volume                     13524(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0980
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21781
_diffrn_reflns_theta_full        24.01
_diffrn_reflns_theta_max         24.01
_diffrn_reflns_theta_min         1.22
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.700
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_correction_T_min  0.7247
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             5904
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         21194
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                10014
_reflns_number_total             21194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja993494c_3.cif
_cod_data_source_block           neu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.0000P] 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^)+(0.0834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115989