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_7009096
_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            'C10.5 H25.5 As0.5 Li0.5 N1.5 P1.5'
_chemical_formula_weight         260.21
_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                108.44(2)
_cell_angle_beta                 90.46(2)
_cell_angle_gamma                108.01(2)
_cell_formula_units_Z            4
_cell_length_a                   9.218(5)
_cell_length_b                   11.182(6)
_cell_length_c                   15.967(8)
_cell_measurement_temperature    180(2)
_cell_volume                     1474.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4457
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.7412
_exptl_absorpt_correction_T_min  0.6466
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.849
_refine_ls_shift/su_mean         0.248
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                3107
_reflns_number_total             3823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908552a.txt
_cod_data_source_block           dw9822
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1474.6(13)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C10.50 H25.50 As0.50 Li0.50 N1.50 P1.50'
_cod_database_code               7009096