A second polymorph of 1,1,4,4-tetramethylpiperazinium pentabromothallate(III)
Linden, Anthony; Petridis, Alexander; James, Bruce D.; Acta Crystallographica Section C 58 (2002) m53–m55; doi:10.1107/S0108270101019746

data_2012464
_publ_section_title
;
 A second polymorph of 1,1,4,4-tetramethylpiperazinium
 pentabromothallate(III)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m53
_journal_page_last               m55
_journal_paper_doi               10.1107/S0108270101019746
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C8 H20 N2) [Tl Br5]'
_chemical_formula_moiety         'C8 H20 N2 2+, Br5 Tl 2-'
_chemical_formula_sum            'C8 H20 Br5 N2 Tl'
_chemical_formula_weight         748.15
_chemical_melting_point          495
_chemical_name_systematic
;
1,1,4,4-tetramethylpiperazinium pentabromothallate(III)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.3928(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0822(3)
_cell_length_b                   9.2422(2)
_cell_length_c                   13.2718(2)
_cell_measurement_reflns_used    2872
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      36.4
_cell_measurement_theta_min      2.9
_cell_volume                     1796.57(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1999)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
'\f scans, and \w scans with \q offsets (\q OK? or \k ?)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .080
_diffrn_reflns_av_sigmaI/netI    .0399
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18998
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.09
_exptl_absorpt_correction_T_max  .105
_exptl_absorpt_correction_T_min  .074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .21
_refine_diff_density_max         2.22
_refine_diff_density_min         -2.26
_refine_ls_extinction_coef       .00183(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         2740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          .0349
_refine_ls_R_factor_gt           .0292
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0247P)^2^+10.0125P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0660
_refine_ls_wR_factor_ref         .0678
_reflns_number_gt                2467
_reflns_number_total             2740
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1524.cif
_cod_data_source_block           Ib
_cod_original_cell_volume        1796.56(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012464
_cod_database_fobs_code          2012464