Comparative refinement of correct and incorrect structural models of tetrabutylammonium tetrabutylborate – pitfalls arising from poor-quality data
Stilinović, Vladimir; Kaitner, Branko; Acta Crystallographica Section A Foundations of Crystallography 66 (2010) 441–445; doi:10.1107/S0108767310013814

data_2019371
_publ_section_title
;
 Comparative refinement of correct and incorrect structural models of
 tetrabutylammonium tetrabutylborate -- pitfalls arising from poor-quality
 data
;
_journal_coeditor_code           ZM5071
_journal_issue                   4
_journal_name_full
'Acta Crystallographica Section A Foundations of Crystallography'
_journal_page_first              441
_journal_page_last               445
_journal_paper_doi               10.1107/S0108767310013814
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C16 H36 N, C16 H36 B'
_chemical_formula_sum            'C32 H72 B N'
_chemical_formula_weight         481.72
_chemical_name_systematic
;
 Tetrabutylammonium Tetrabutylborate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.958(5)
_cell_length_b                   18.958(5)
_cell_length_c                   10.624(5)
_cell_measurement_reflns_used    145
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      4.6
_cell_volume                     3818(2)
_computing_cell_refinement
;
CrysAlis RED 170 (Oxford Diffraction Poland Sp., 2003)
;
_computing_data_collection
;
CrysAlis CCD 170 (Oxford Diffraction Poland Sp., 2003)
;
_computing_data_reduction
;
CrysAlis RED 170 (Oxford Diffraction Poland Sp., 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.172
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12512
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    0.046
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.744
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.744
_refine_ls_R_factor_all          0.3277
_refine_ls_R_factor_gt           0.0807
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1944
_refine_ls_wR_factor_ref         0.2554
_reflns_number_gt                408
_reflns_number_total             2075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zm5071sup1.cif
_cod_data_source_block           IMo
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2019371