Cyclooctatetraene Complexes of Yttrium and the Lanthanides with Bis(phosphinimino)methanides: Synthesis, Structure, and Hydroamination/Cyclization Catalysis
Panda, Tarun K.; Zulys, Agustino; Gamer, Michael T.; Roesky, Peter W.; Organometallics 24 (2005) 2197–2202; doi:10.1021/om0491138

data_1100886
_publ_section_title
;
 Cyclooctatetraene Complexes of Yttrium and the Lanthanides with
 Bis(phosphinimino)methanides: Synthesis, Structure, and
 Hydroamination/Cyclization Catalysis
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2197
_journal_page_last               2202
_journal_paper_doi               10.1021/om0491138
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C41.5 H52 Lu N2 P2 Si2'
_chemical_formula_weight         871.94
_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-97
_cell_angle_alpha                93.619(5)
_cell_angle_beta                 92.852(5)
_cell_angle_gamma                99.437(5)
_cell_formula_units_Z            2
_cell_length_a                   9.351(2)
_cell_length_b                   9.500(2)
_cell_length_c                   22.700(5)
_cell_measurement_temperature    173(2)
_cell_volume                     1981.7(7)
_computing_molecular_graphics    'Diamond 2.1 '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'area detector'
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23438
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         0.90
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    2.663
_exptl_absorpt_correction_T_max  0.345
_exptl_absorpt_correction_T_min  0.19044
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.661
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         11918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.3361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                10971
_reflns_number_total             11918
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4060421
_cod_data_source_file            om0491138si20041116_113831.cif
_cod_data_source_block           1e
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C41.50 H52 Lu N2 P2 Si2'
_cod_database_code               1100886