Hydrogen-bonded cubanes in the crystal structure of 2,6-di(Pri)aniline hydrochloride and their inorganic analogues [M2+(2,6-di(Pri)C6H5N2-)]4 (M = Sn, Pb)
Bond, Andrew D.; Doyle, Emma L.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2324–2325; doi:10.1039/b307400e

data_7113439
_publ_section_title
;
 Hydrogen-bonded cubanes in the crystal structure of 2,6-di(Pri)aniline
 hydrochloride and their inorganic analogues [M2+(2,6-di(Pri)C6H5N2-)]4
 (M = Sn, Pb)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   18
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2324
_journal_page_last               2325
_journal_paper_doi               10.1039/b307400e
_journal_year                    2003
_chemical_formula_moiety         '4 (C12 H20 N +), 4 Cl -, (C4 H8 O)0.5'
_chemical_formula_sum            'C50 H84 Cl4 N4 O0.5'
_chemical_formula_weight         891.01
_chemical_melting_point          479
_chemical_name_common
;
2,6-di-isopropyl-aniline hydrochloride, thf solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 plus manual editing'
_cell_angle_alpha                81.907(2)
_cell_angle_beta                 80.031(2)
_cell_angle_gamma                69.019(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5989(4)
_cell_length_b                   14.6215(5)
_cell_length_c                   17.3570(6)
_cell_measurement_reflns_used    18412
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2697.01(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28837
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         12290
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.1023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                8630
_reflns_number_total             12290
_reflns_threshold_expression     I>2\s(I)
_cod_duplicate_entry             7104808
_cod_data_source_file            b307400e.txt
_cod_data_source_block           dw0202
_cod_original_cell_volume        2697.01(16)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C50 H84 Cl4 N4 O0.50'
_cod_database_code               7113439