A Lanthanide Phosphinidene Complex: Synthesis, Structure, and Phospha-Wittig Reactivity
Jason D. Masuda; Kimberly C. Jantunen; Oleg V. Ozerov; Kevin J. T. Noonan; Derek P. Gates; Brian L. Scott; Jaqueline L. Kiplinger; Journal of the American Chemical Society 130 (2008) 2408–2409; doi:10.1021/ja7105306

data_4107463
_publ_contact_author_address
;
Los Alamos National Laboratory
MS J514
Los Alamos, NM  87544
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_contact_author_name        'Jaqueline L. Kiplinger'
_publ_section_title
;
 A Lanthanide Phosphinidene Complex: Synthesis, Structure, and
 Phospha-Wittig Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2408
_journal_page_last               2409
_journal_paper_doi               10.1021/ja7105306
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C34 H62 Lu N P2 Si2'
_chemical_formula_weight         777.94
_chemical_name_systematic
; 
 ? 
;
_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                93.120(2)
_cell_angle_beta                 109.3100(10)
_cell_angle_gamma                112.1280(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8412(16)
_cell_length_b                   12.0344(17)
_cell_length_c                   15.568(2)
_cell_measurement_temperature    141(2)
_cell_volume                     1898.4(4)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17078
_diffrn_reflns_theta_full        24.59
_diffrn_reflns_theta_max         24.59
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.770
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                5125
_reflns_number_total             6353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7105306-file002_1.cif
_cod_data_source_block           apx525
_cod_original_cell_volume        1898.3(5)
_cod_database_code               4107463