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_4108075
_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            'C43 H60 N3 O5 P3 W2'
_chemical_formula_weight         1159.55
_chemical_name_common            (CO)5W(cyclo-P3)W(N[iPr]Ar)3
_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                77.231(3)
_cell_angle_beta                 75.225(3)
_cell_angle_gamma                67.525(3)
_cell_formula_units_Z            2
_cell_length_a                   11.350(2)
_cell_length_b                   14.150(3)
_cell_length_c                   16.557(3)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2353.1(8)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44584
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_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    5.031
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.5191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.462
_refine_diff_density_min         -3.862
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         12603
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0149P)^2^+22.2758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                9954
_reflns_number_total             12603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802080m-file002.cif
_cod_data_source_block           06209
_cod_original_cell_volume        2352.9(8)
_cod_database_code               4108075