Solid-state synthesis of mixed trihalides via reversible absorption of dihalogens by non porous onium salts
Meazza, Lorenzo; Martí-Rujas, Javier; Terraneo, Giancarlo; Castiglioni, Chiara; Milani, Alberto; Pilati, Tullio; Metrangolo, Pierangelo; Resnati, Giuseppe; CrystEngComm 13 (2011) 4427–; doi:10.1039/c1ce05050h

data_7206177
_publ_section_title
;
 Solid-state synthesis of mixed trihalides via reversible absorption of
 dihalogens by non porous onium salts
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              4427
_journal_paper_doi               10.1039/c1ce05050h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C12 H30 N2 2+, 2(Br 1-), 2(H2 O)'
_chemical_formula_sum            'C12 H34 Br2 N2 O2'
_chemical_formula_weight         398.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.824(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3339(13)
_cell_length_b                   18.292(3)
_cell_length_c                   7.0915(12)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.94
_cell_volume                     900.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, L.J. (1997) Jour. Appl. Cryst. 30, 565)
Mercury (Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E.,
Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006).
J. Appl. Cryst. 39, 453-457
;
_computing_publication_material  SHELXTL
_computing_structure_refinement
'SHELXL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122)'
_computing_structure_solution
;
SIR2002 (Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003).
J. Appl. Cryst. 36, 1103.)
;
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            30772
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.24
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    4.501
_exptl_absorpt_correction_T_max  0.4005
_exptl_absorpt_correction_T_min  0.2766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       table
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0202P)^2^+0.4646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                2412
_reflns_number_total             2604
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1ce05050h.txt
_cod_data_source_block           jm044
_cod_original_cell_volume        900.4(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7206177