A synthetic and structural study of the formation of cyclic [(RP)nE]− anions and Zintl compounds using E(NMe2)3 (E = As, Sb)
Bashall, Alan; Beswick, Michael A.; Choi, Nick; Hopkins, Alexander D.; Kidd, Sara J.; Lawson, Yvonne G.; Mosquera, Marta E. G.; McPartlin, Mary; Raithby, Paul R.; Wheatley, Andrew A. E. H.; Wood, Jody A.; Wright, Dominic S.; Journal of the Chemical Society, Dalton Transactions  (2000) 479–; doi:10.1039/a908552a

data_7009098
_publ_section_title
;
 A synthetic and structural study of the formation of cyclic
 [(RP)nE]&#x2212; anions and Zintl compounds using E(NMe2)3
 (E&#x2005;=&#x2005;As, Sb)
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              479
_journal_paper_doi               10.1039/a908552a
_journal_year                    2000
_chemical_formula_sum            'C43.5 H73 As Li N2 O P3'
_chemical_formula_weight         814.81
_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                100.07(2)
_cell_angle_beta                 112.31(3)
_cell_angle_gamma                79.90(3)
_cell_formula_units_Z            2
_cell_length_a                   12.518(6)
_cell_length_b                   17.347(4)
_cell_length_c                   11.166(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      8
_cell_volume                     2192.8(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10544
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.8376
_exptl_absorpt_correction_T_min  0.7702
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10082
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          1.151
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                7622
_reflns_number_total             10082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908552a.txt
_cod_data_source_block           dw9912
_cod_original_cell_volume        2192.8(14)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C43.50 H73 As Li N2 O P3'
_cod_database_code               7009098