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_7009097
_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            'C28 H59 As Li N4 O P3'
_chemical_formula_weight         642.56
_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
_cell_angle_alpha                71.11(3)
_cell_angle_beta                 73.79(3)
_cell_angle_gamma                64.61(3)
_cell_formula_units_Z            2
_cell_length_a                   11.651(2)
_cell_length_b                   12.638(3)
_cell_length_c                   13.991(3)
_cell_measurement_temperature    180(2)
_cell_volume                     1737.0(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       NoniusKappaCCD
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11462
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.142
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   0.937
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      0.937
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         -0.073
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1173
_refine_ls_wR_factor_obs         0.0901
_reflns_number_observed          6276
_reflns_number_total             7903
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908552a.txt
_cod_data_source_block           dw9936
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1737.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009097