P2Addition to Terminal Phosphide M\τbP Triple Bonds: A Rational Synthesis of cyclo-P3 Complexes
Nicholas A. Piro; Christopher C. Cummins; Journal of the American Chemical Society 130 (2008) 9524–9535; doi:10.1021/ja802080m

data_4108076
_publ_contact_author_address
;Department of Chemistry
Massachusetts Institute of Technology
77 Massachusetts Avenue, Room 6-435
Cambridge, MA  02139-4307 (USA)
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_fax         617-258-5700
_publ_contact_author_name        'Christopher C. Cummins'
_publ_contact_author_phone       617-253-5332
_publ_section_title
;
 P2Addition to Terminal Phosphide M\\tbP Triple Bonds: A Rational
 Synthesis of cyclo-P3 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9524
_journal_page_last               9535
_journal_paper_doi               10.1021/ja802080m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C59 H76 N3 Na Nb O11 P3 W2'
_chemical_formula_weight         1579.74
_chemical_name_common
'{Et2ONa}{[W(CO)5]2(cyclo-P3)Nb(N[Np]Ar)3} (C6H6)'
_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                106.235(4)
_cell_angle_beta                 91.068(4)
_cell_angle_gamma                94.536(4)
_cell_formula_units_Z            2
_cell_length_a                   12.145(3)
_cell_length_b                   13.565(3)
_cell_length_c                   22.695(6)
_cell_measurement_reflns_used    7638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     3575.3(15)
_computing_cell_refinement       'SAINT 7 (Bruker-AXS, 2005)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 7 (Bruker-AXS, 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62023
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.5419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14086
_refine_ls_number_restraints     797
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+2.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                9270
_reflns_number_total             14086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802080m-file003.cif
_cod_data_source_block           06215
_cod_original_cell_volume        3575.5(15)
_cod_database_code               4108076