Triple-Bond Reactivity of an AsP Complex Intermediate: Synthesis Stemming from Molecular Arsenic, As4
Heather A. Spinney; Nicholas A. Piro; Christopher C. Cummins; Journal of the American Chemical Society 131 (2009) 16233–16243; doi:10.1021/ja906550h

data_4105308
_publ_section_title
;
 Triple-Bond Reactivity of an AsP Complex Intermediate: Synthesis Stemming
 from Molecular Arsenic, As4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16233
_journal_page_last               16243
_journal_paper_doi               10.1021/ja906550h
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C61 H99 As N4 Nb O P'
_chemical_formula_weight         1103.24
_chemical_name_common            (Mes*NPAs)Nb(N[Np]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                69.8760(10)
_cell_angle_beta                 78.4010(10)
_cell_angle_gamma                87.0670(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7490(5)
_cell_length_b                   16.4700(7)
_cell_length_c                   17.3444(7)
_cell_measurement_reflns_used    5629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.23
_cell_volume                     3086.4(2)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60657
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.8264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         15903
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0530P)^2^+0.4386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                11893
_reflns_number_total             15903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906550h_si_001_2.cif
_cod_data_source_block           06112
_cod_database_code               4105308