Crystalline Salts of Na-and K-(Alkalides) that Are Stable at Room Temperature
Jineun Kim; Andrew S. Ichimura; Rui H. Huang; Mikhail Redko; Richard C. Phillips; James E. Jackson; James L. Dye; Journal of the American Chemical Society 121 (1999) 10666–10667; doi:10.1021/ja992667v

data_4116599
_publ_section_title
;
 Crystalline Salts of Na-and K-(Alkalides) that Are Stable at Room
 Temperature
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10666
_journal_page_last               10667
_journal_paper_doi               10.1021/ja992667v
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C24 H54 N8'
_chemical_formula_weight         454.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.555(2)
_cell_length_b                   14.555(2)
_cell_length_c                   11.446(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2099.9(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8164
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.067
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_F_000             762
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(611)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.982
_refine_ls_goodness_of_fit_obs   1.003
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2233
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.981
_refine_ls_restrained_S_obs      1.003
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_obs          0.0720
_refine_ls_shift/esd_max         0.738
_refine_ls_shift/esd_mean        0.182
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1906P)^2^+1.5472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2505
_refine_ls_wR_factor_obs         0.2299
_reflns_number_observed          1815
_reflns_number_total             2233
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja992667v_1.cif
_cod_data_source_block           aza222
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1906P)^2^+1.5472P] 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^)+(0.1906P)^2^+1.5472P] 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        2100.0(6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4116599