Synthesis, Structure, and Reactivity of Unsolvated Triple-Decked Bent Metallocenes of Divalent Europium and Ytterbium
Evans, William J.; Johnston, Matthew A.; Greci, Michael A.; Ziller, Joseph W.; Organometallics 18 (1999) 1460–; doi:10.1021/om980762r

data_4077747
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Unsolvated Triple-Decked Bent
 Metallocenes of Divalent Europium and Ytterbium
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1460
_journal_paper_doi               10.1021/om980762r
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C28 H38 Yb2'
_chemical_formula_weight         720.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                114.772(7)
_cell_angle_beta                 93.948(11)
_cell_angle_gamma                90.803(14)
_cell_formula_units_Z            4
_cell_length_a                   13.338(2)
_cell_length_b                   13.549(2)
_cell_length_c                   15.815(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    163
_cell_measurement_theta_max      11.85
_cell_measurement_theta_min      4.96
_cell_volume                     2586.0(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        CARESS
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      163
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11704
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    7.200
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.1352
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.966
_refine_diff_density_min         -4.280
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       0.0006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         11224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_obs          0.0604
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+2.1362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1777
_refine_ls_wR_factor_obs         0.1607
_reflns_number_observed          8750
_reflns_number_total             11224
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980762r.cif
_cod_data_source_block           maj5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+2.1362P] 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^)+(0.1342P)^2^+2.1362P] 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        2585.9(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077747