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_4108079
_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            'C62.5 H81 N3 Nb O11 P3 W2'
_chemical_formula_weight         1603.82
_chemical_name_common            '[W(CO)5]2(AdC(O)P3)Nb(N[Np]Ar)3 (C5H10)0.5'
_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                 106.2100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9056(12)
_cell_length_b                   21.2534(18)
_cell_length_c                   23.425(2)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.45
_cell_volume                     6647.8(10)
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            144330
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.751
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.4540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2005)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       plate
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         18654
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0161P)^2^+8.7211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                15728
_reflns_number_total             18654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802080m-file006.cif
_cod_data_source_block           06237
_cod_original_cell_volume        6647.7(10)
_cod_original_formula_sum        'C62.50 H81 N3 Nb O11 P3 W2'
_cod_database_code               4108079