Novel Anionic Lanthanocene Amide Complexes: Syntheses and X-ray Crystal Structures of [Na(THF)2(μ-η5:η5-MeC5H4)2Ln(NPh2)2]n(Ln = Sm, Er)
Wang, Yaorong; Shen, Qi; Xue, Feng; Yu, Kaibei; Organometallics 19 (2000) 357–; doi:10.1021/om9906215

data_4077659
_publ_section_title
;
 Novel Anionic Lanthanocene Amide Complexes:&#x00A0; Syntheses and X-ray
 Crystal Structures of [Na(THF)2(\m-\h5:\h5-MeC5H4)2Ln(NPh2)2]n(Ln = Sm,
 Er)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              357
_journal_paper_doi               10.1021/om9906215
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C44 H50 N2 Na O2 Sm'
_chemical_formula_weight         812.20
_chemical_name_systematic
; 
 ? 
;
_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                 101.83(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.006(1)
_cell_length_b                   22.009(2)
_cell_length_c                   20.763(2)
_cell_measurement_reflns_used    '161 from 4 still frames'
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4028.1(7)
_computing_cell_refinement       'bioteX 1.0 (MSC, 1995)'
_computing_data_collection       'bioteX 1.0 (MSC, 1995)'
_computing_data_reduction        'bioteX 1.0 (MSC, 1995)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Rigaku RAXIS IIc'
_diffrn_measurement_method
;
Data was collected to 0.82\%A and 85% completeness by taking
54 oscillation frames in the range of 0 - 162\%, \D\f = 3\%,
8 min. per frame.  Crystal to detector distance is 77.938 mm,
background level -100.
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator powered at 50kV / 50mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12175
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.505
_exptl_absorpt_correction_T_max  1.093
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0071(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6665
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+1.2323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1393
_refine_ls_wR_factor_ref         0.1438
_reflns_number_gt                6239
_reflns_number_total             6665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9906215.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        4028.1(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077659