Pitfalls of a structure determination: The structure of closo-9-[4-(dibenzylamino)phenyl]-1,2-dicarbadodecaborane(12)
Milewski, Max; Caminade, Anne-Marie; Hey-Hawkins, Evamarie; Lönnecke, Peter; Acta Crystallographica Section E Crystallographic Communications 78 (2022) –; doi:10.1107/S205698902201043X

data_2022692
_publ_section_title
;
 Pitfalls of a structure determination: The structure of
 closo-9-[4-(dibenzylamino)phenyl]-1,2-dicarbadodecaborane(12)
;
_journal_coeditor_code           JQ2023
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S205698902201043X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C22 H29 B10 N'
_chemical_formula_moiety         'C22 H29 B10 N'
_chemical_formula_sum            'C22 H29 B10 N'
_chemical_formula_weight         415.56
_chemical_name_systematic
;
<i>closo</i>-9-[4-(Dibenzylamino)phenyl]-1,2-dicarbadodecaborane(12)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0128(2)
_cell_length_b                   27.1423(4)
_cell_length_c                   13.9114(3)
_cell_measurement_reflns_used    15129
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      31.7300
_cell_measurement_theta_min      2.7330
_cell_volume                     4632.07(15)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
DIAMOND (Crystal Impact GbR, 2022)
;
_computing_publication_material
;
WINGX (Farrugia, 2012)
;
_computing_structure_refinement
;
<i>SHELXL2018-3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018-2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            76840
_diffrn_reflns_theta_full        30.510
_diffrn_reflns_theta_max         31.977
_diffrn_reflns_theta_min         2.160
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         15117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+0.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                9789
_reflns_number_total             15117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jq2023sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022692
_shelx_res_checksum              26689
_cod_database_fobs_code 2022692