NO-Anion Trapped in a Molecular Oxide Bowl
N. Kawanami; T. Ozeki; A. Yagasaki; Journal of the American Chemical Society 122 (2000) 1239–1240; doi:10.1021/ja993539+

data_4115919
_publ_section_title
;
 NO-Anion Trapped in a Molecular Oxide Bowl
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1239
_journal_page_last               1240
_journal_paper_doi               10.1021/ja993539+
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C44 H108 Cl8 N6 O33 V12'
_chemical_formula_weight         2144.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.3979(4)
_cell_length_b                   19.3979(4)
_cell_length_c                   11.3278(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    125
_cell_volume                     4262.41(17)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    Chemray
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35282
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8818
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       'tetragonal pillar'
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                5959
_reflns_number_total             6461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9935392B.cif
_cod_data_source_block           v12
_cod_database_code               4115919