Direct synthesis of the 1,2,3-[C6H4P...P...P]- anion, isoelectronic with the indenyl anion [C6H4CH...CH...CH]-.
García, Felipe; Less, Robert J; Naseri, Vesal; McPartlin, Mary; Rawson, Jeremy M; Sancho Tomas, Maria; Wright, Dominic S; Chemical communications (Cambridge, England)  (2008) 859–861; doi:10.1039/b718425e

data_7102902
_publ_section_title
;
 Direct synthesis of the 1,2,3-[C6H4P...P...P]- anion, isoelectronic
 with the indenyl anion [C6H4CH...CH...CH]-.
;
_journal_issue                   7
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              859
_journal_page_last               861
_journal_paper_doi               10.1039/b718425e
_journal_year                    2008
_chemical_formula_moiety         '3(C16 H32 Li O8), Sb11'
_chemical_formula_sum            'C48 H96 Li3 O24 Sb11'
_chemical_formula_weight         2417.32
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.138(2)
_cell_length_b                   21.138(2)
_cell_length_c                   32.330(2)
_cell_measurement_reflns_used    4653
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.02
_cell_volume                     12510.2(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 0.488
_diffrn_measured_fraction_theta_max 0.488
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            2555
_diffrn_reflns_theta_full        22.80
_diffrn_reflns_theta_max         22.80
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0653P)^2^+1065.7550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                1568
_reflns_number_total             2023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718425e.txt
_cod_data_source_block           dw0752
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7102902