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_4107464
_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            'C84 H118 Lu2 N2 P6'
_chemical_formula_weight         1691.56
_chemical_name_systematic
; 
 ? 
;
_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                 110.892(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.993(3)
_cell_length_b                   24.746(4)
_cell_length_c                   17.489(3)
_cell_measurement_temperature    141(2)
_cell_volume                     8084(2)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 5.10 (Bruker, 1997)'
_computing_publication_material  'SHELXTL 5.10 (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       '\f 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  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            77845
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.590
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.7799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         14243
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                10222
_reflns_number_total             14243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7105306-file002_2.cif
_cod_data_source_block           xpl041s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4107464