The 18-crown-6 potassium salt of a Meissenheimer anion, [K(C~7~H~3~Cl~3~N~3~O~6~)(C~12~H~24~O~6~)]
Barnes, John C.; Main, Jenifer; Paton, John D.; Acta Crystallographica Section C 50 (1994) 1247–1249; doi:10.1107/S010827019400226X

data_2009976
_publ_section_title
;
 The 18-crown-6 potassium salt of a Meissenheimer anion,
 [K(C~7~H~3~Cl~3~N~3~O~6~)(C~12~H~24~O~6~)]
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1247
_journal_page_last               1249
_journal_paper_doi               10.1107/S010827019400226X
_journal_volume                  50
_journal_year                    1994
_chemical_formula_structural     'C12 H24 K O6 , C7 H9 Cl3 N3 O6'
_chemical_formula_sum            'C19 H27 Cl3 K N3 O12'
_chemical_formula_weight         634.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                72.59(3)
_cell_angle_beta                 61.72(3)
_cell_angle_gamma                63.44(2)
_cell_formula_units_Z            2
_cell_length_a                   11.676(3)
_cell_length_b                   11.845(3)
_cell_length_c                   13.110(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     1419.4(8)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_molecular_graphics    'PLUTON92 (Spek, 1992)'
_computing_structure_refinement
;
SHELX-76 (Sheldrick, 1976) with SHELXL-93 (Sheldrick, 1994) used for last
cycles and preparation of CIF file
;
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.2423
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5581
_diffrn_reflns_theta_max         23.97
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plates
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.334
_refine_ls_goodness_of_fit_obs   0.332
_refine_ls_hydrogen_treatment
;
U refined for groups of H, position and U refined for H21'
;
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.334
_refine_ls_restrained_S_obs      0.332
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.1000P)^2^+0.0000P]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1387
_refine_ls_wR_factor_obs         0.0930
_reflns_number_observed          1975
_reflns_number_total             4369
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            li1100.cif
_cod_data_source_block           hkm
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1419.4(7)
_cod_database_code               2009976