Lithium bis(tetramethyllammonium) hexanitrocobaltate(III) at 113 and 293 K
Adovasio, Victor; Lina, Fausto; Nardelli, Mario; Pelizzi, Giancarlo; Acta Crystallographica Section C 50 (1994) 871–874; doi:10.1107/S0108270193011588

data_2009794
_publ_section_title
;
 Lithium bis(tetramethyllammonium) hexanitrocobaltate(III) at 113 and
 293 K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              871
_journal_page_last               874
_journal_paper_doi               10.1107/S0108270193011588
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical     'Li 1+,2C4 H12 N1 1+, [Co1 (N1 O2)6] 3-'
_chemical_formula_moiety         'Li 1+,2(C4 H12 N1 1+), Co1 N6 O12 3-'
_chemical_formula_sum            'C8 H24 Co Li N8 O12'
_chemical_formula_weight         490.20
_chemical_name_systematic
;
Litium bis(tetramethylammonium) hexanitrocobaltate(III)
;
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 m 1'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   8.8560(10)
_cell_length_b                   8.8560(10)
_cell_length_c                   7.017(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    113.0(10)
_cell_measurement_theta_max      17.39
_cell_measurement_theta_min      11.23
_cell_volume                     476.60(16)
_computing_cell_refinement       'LQPARM (Nardelli & Mangia, 1984)'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics
;
 ORTEP (Johnson, 1965), PLUTO (Motherwell & Clegg, 1976)
;
_computing_publication_material
;
 PARST (Nardelli, 1983), PARSTCIF (Nardelli, 1992)
;
_computing_structure_refinement  'SHELXL92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      113.0(10)
_diffrn_measurement_device       'ENRAF-NONIUS CAD4 diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus X-ray sealed tube'
_diffrn_radiation_type           'Mo K\a mean'
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0356
_diffrn_reflns_av_sigmaI/netI    .0329
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11116
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_max         75.23
_diffrn_reflns_theta_min         3.94
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_time  160
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    .979
_exptl_absorpt_correction_T_max  .744
_exptl_absorpt_correction_T_min  .732
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_description
;
 small pseudo octahedra
;
_exptl_crystal_F_000             254
_exptl_crystal_size_max          .55
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .39
_refine_diff_density_max         1.86
_refine_diff_density_min         -1.03
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         3653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_obs          .0292
_refine_ls_shift/esd_max         <0.001
_refine_ls_shift/esd_mean        .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
 calc w = 1/[\s^2^(F~o~^2^) + (0.0291P)^2^ + 0.0822P] where
   P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_obs         .0765
_reflns_number_observed          3391
_reflns_number_total             3662
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            mu1078.cif
_cod_data_source_block           113K
_cod_original_cell_volume        476.6(2)
_cod_database_code               2009794