Direct access to [(Mes*P)2As]-, a 1,3-diphosphaarsa-2-allyl anion, isoelectronic with the allyl anion (Mes* = 2,4,6^-t^Bu3C6H2)
Lily S. H. Dixon; Lucy K. Allen; Robert J. Less; Dominic S. Wright; Chem.Commun. 50 (2014) 3007–; doi:10.1039/c3cc49627a

data_7112082
_publ_section_title
;
 Direct access to [(Mes*P)2As]-, a 1,3-diphosphaarsa-2-allyl anion,
 isoelectronic with the allyl anion (Mes* = 2,4,6^-t^Bu3C6H2)
;
_journal_name_full               Chem.Commun.
_journal_page_first              3007
_journal_paper_doi               10.1039/c3cc49627a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C44 H81 As1 Li1 N3 P2, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H88 As Li N3 P2'
_chemical_formula_weight         839.00
_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                 103.881(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5585(3)
_cell_length_b                   19.2337(3)
_cell_length_c                   18.1616(4)
_cell_measurement_reflns_used    15450
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     5615.21(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31427
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         9788
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1396P)^2^+6.6899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2213
_refine_ls_wR_factor_ref         0.2471
_reflns_number_gt                6500
_reflns_number_total             9788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49627a2.cif
_cod_data_source_block           dw1370
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7112082