Synthesis, Structure, and Dynamics of Tris(η5-cyclopentadienyl)lanthanides and Bis(η5-cyclopentadienyl)[bis(trimethylsilyl)amido]cerium(III)
Baisch, Ulrich; Pagano, Sandro; Zeuner, Martin; Schmedt auf der Günne, Jörn; Oeckler, Oliver; Schnick, Wolfgang; Organometallics 25 (2006) 3027–; doi:10.1021/om060226w

data_4075335
_publ_contact_author
;
        Prof. Wolfgang Schnick
        Department Chemie und Biochemie
        Ludwig-Maximilians-Universit\"at Mueunchen
        Butenandtstrasse 5 - 13 (D)
        D 81377 Mueunchen
        Germany
;
_publ_section_title
;
 Synthesis, Structure, and Dynamics of
 Tris(\h5-cyclopentadienyl)lanthanides and
 Bis(\h5-cyclopentadienyl)[bis(trimethylsilyl)amido]cerium(III)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3027
_journal_paper_doi               10.1021/om060226w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C15 H15 Ce1'
_chemical_formula_sum            'C15 H15 Ce'
_chemical_formula_weight         335.39
_chemical_melting_point          ?
_chemical_name_common            Ceriumocene
_chemical_name_systematic        tris-cyclopentadienyl-cerium(III)
_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                 93.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.121(3)
_cell_length_b                   9.6696(19)
_cell_length_c                   16.593(3)
_cell_measurement_reflns_used    5689
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.7
_cell_volume                     2422.7(8)
_computing_cell_refinement       'STOE IPDS'
_computing_data_collection       'STOE IPDS'
_computing_data_reduction        'STOE IPDS'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.662
_diffrn_measured_fraction_theta_max 0.657
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'STOE IPDS'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9921
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.76
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_voltage           50_kV
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  0.59284
_exptl_absorpt_correction_T_min  0.41817
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Prep Correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+17.7046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                1964
_reflns_number_total             3249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060226wsi20060311_015918.cif
_cod_data_source_block
;
;
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

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 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C15 H15 Ce1'
_cod_database_code               4075335
_kl_diffrn_detector_area_plate_dist 50.0_mm
_kl_diffrn_detector_area_phi_incr 0.9
_kl_diffrn_detector_area_expos_time 10.0_min
_kl_diffrn_detector_area_profile_min 9
_kl_diffrn_detector_area_profile_max 11
_kl_diffrn_detector_area_phi_start 0.0
_kl_diffrn_detector_area_phi_end 180.0
_kl_diffrn_detector_area_eff_mos_spread 0.009