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_7112083
_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         'C36 H58 As1 P2 1-, 2(C8 H16 O4), Li 1+'
_chemical_formula_sum            'C52 H90 As Li O8 P2'
_chemical_formula_weight         987.04
_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                90.751(3)
_cell_angle_beta                 91.460(3)
_cell_angle_gamma                115.777(3)
_cell_formula_units_Z            2
_cell_length_a                   13.217(1)
_cell_length_b                   14.553(2)
_cell_length_c                   16.489(2)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      37.5
_cell_measurement_theta_min      2.6
_cell_volume                     2854.1(6)
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_collection       'Bruker software package, narrow-frames'
_computing_data_reduction
;
 Bruker SAINT software package, narrow frame algorithm
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15528
_diffrn_reflns_theta_full        33.40
_diffrn_reflns_theta_max         33.40
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (SADABS) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.1252
_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^)+(0.0275P)^2^+104.0250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2521
_refine_ls_wR_factor_ref         0.2585
_reflns_number_gt                1938
_reflns_number_total             2186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49627a2.cif
_cod_data_source_block           dw1372
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112083