New Dinuclear 5-ansa-Lanthanocene Derivatives. Crystal Structures of [Ln{2,6-(CH2C5H4)2C5H3N}μ-O2SOCF3]2(Ln = Nd, Y, Yb) and a VT Solution NMR (1H,19F) Study of the Fluxional Yttrium Homologue
Paolucci, Gino; Zanon, Jacopo; Lucchini, Vittorio; Damrau, Wulf-Erich; Siebel, Eric; Fischer, R. Dieter; Organometallics 21 (2002) 1088–; doi:10.1021/om0104868

data_4076626
_publ_section_title
;
 New Dinuclear 5-ansa-Lanthanocene Derivatives. Crystal Structures of
 [Ln{2,6-(CH2C5H4)2C5H3N}\m-O2SOCF3]2(Ln = Nd, Y, Yb) and a VT Solution
 NMR (1H,19F) Study of the Fluxional Yttrium Homologue
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1088
_journal_paper_doi               10.1021/om0104868
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C18.5 H17 Cl2 F3 N Nd O3 S'
_chemical_formula_weight         605.53
_chemical_name_systematic
;
Di[2,6-bis(\n^5^-cyclopentadienylmethylen)pyridin(\m^2^-triflate)Neodyme(III)]
;
_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           SHELXL
_cell_angle_alpha                91.86(3)
_cell_angle_beta                 90.51(3)
_cell_angle_gamma                107.71(3)
_cell_formula_units_Z            4
_cell_length_a                   12.438(3)
_cell_length_b                   13.320(3)
_cell_length_c                   13.950(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.5
_cell_volume                     2200.0(9)
_computing_cell_refinement       'P21 (J.Kopf, D. Abeln, 1993)'
_computing_data_collection       'P21 (J.Kopf, D. Abeln, 1993)'
_computing_data_reduction        'P21 (J.Kopf, D. Abeln, 1993)'
_computing_molecular_graphics    'XP, Bruker Analytik 1997'
_computing_publication_material  'PLATON 95, (Speck 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Hilger & Watts Y290'
_diffrn_measurement_method       2\q-\q
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15068
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.742
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       'transparent blocs'
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0023(3)
_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_all   0.743
_refine_ls_goodness_of_fit_obs   0.716
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         12899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.743
_refine_ls_restrained_S_obs      0.716
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_obs          0.0330
_refine_ls_shift/esd_max         4.055
_refine_ls_shift/esd_mean        0.157
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+3.9468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1142
_refine_ls_wR_factor_obs         0.1018
_reflns_number_observed          11080
_reflns_number_total             12900
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0104868.cif
_cod_data_source_block           dam7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+3.9468P] 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^)+(0.1149P)^2^+3.9468P] 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        2200.0(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H17 Cl2 F3 N Nd O3 S'
_cod_database_code               4076626