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_7206180
_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(Cl I2 1-)'
_chemical_formula_sum            'C12 H30 Cl2 I4 N2'
_chemical_formula_weight         780.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 91.388(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.361(3)
_cell_length_b                   7.5412(12)
_cell_length_c                   7.1251(10)
_cell_measurement_reflns_used    2980
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      2.85
_cell_volume                     1201.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122)'
_computing_structure_solution
;
SUPERFLIP (L. Palatinus and G. Chapuis (2007) J. Appl. Cryst 40, 786-790'
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7261
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    5.407
_exptl_absorpt_correction_T_max  0.5568
_exptl_absorpt_correction_T_min  0.4418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       table
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+1.5366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                1453
_reflns_number_total             1910
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1ce05050h.txt
_cod_data_source_block           mz127
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'NOREF' changed to 'noref'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7206180