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_4077746
_publ_section_title
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 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            'C35 H46 Eu2'
_chemical_formula_weight         770.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.856(6)
_cell_length_b                   15.220(6)
_cell_length_c                   17.399(6)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    153
_cell_measurement_theta_max      15.65
_cell_measurement_theta_min      5.80
_cell_volume                     3140(2)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3456
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_count 99
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_T_max  0.1022
_exptl_absorpt_correction_T_min  0.0648
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.226
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.269
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.255
_refine_ls_goodness_of_fit_obs   1.315
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_restrained_S_obs      1.315
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         1.310
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+33.5493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1665
_refine_ls_wR_factor_obs         0.1519
_reflns_number_observed          2762
_reflns_number_total             3456
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980762r.cif
_cod_data_source_block           maj4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+33.5493P] 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^)+(0.0653P)^2^+33.5493P] 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        3139.9(23)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4077746