Bis(1,3,4-trimethylpyridinium) tetrachloridocuprate(II) and bis(1,3,4-trimethylpyridinium) tetrabromidocuprate(II): an examination of the <i>A</i>~2~Cu<i>X</i>~4~ <i>Fdd</i>2 structure type
Bond, Marcus R.; Acta Crystallographica Section C 65 (2009) m279–m283; doi:10.1107/S0108270109023968

data_2017271
_publ_section_title
;
 Bis(1,3,4-trimethylpyridinium) tetrachloridocuprate(II) and
 bis(1,3,4-trimethylpyridinium) tetrabromidocuprate(II): an examination
 of the <i>A</i>~2~Cu<i>X</i>~4~ <i>Fdd</i>2 structure type
;
_journal_coeditor_code           SU3035
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m279
_journal_page_last               m283
_journal_paper_doi               10.1107/S0108270109023968
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C8 H12 N)2 [Cu Br4]'
_chemical_formula_moiety         '2C8 H12 N + , Br4 Cu 2-'
_chemical_formula_sum            'C16 H24 Br4 Cu N2'
_chemical_formula_weight         627.55
_chemical_name_systematic
;
bis(1,3,4-trimethylpyridinium) tetrabromidocuprate(II)
;
_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'
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.8540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8882(4)
_cell_length_b                   14.8736(3)
_cell_length_c                   8.37720(10)
_cell_measurement_reflns_used    17042
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2212.93(7)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL DENZO and SCALEPACK (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37761
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.7
_exptl_absorpt_coefficient_mu    8.21
_exptl_absorpt_correction_T_max  0.5336
_exptl_absorpt_correction_T_min  0.2417
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(grid of 8 x 8 x 8 sampling points; Software?)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.46
_refine_ls_extinction_coef       0.0033(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.07
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.6550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3469
_reflns_number_total             5071
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su3035.cif
_cod_data_source_block           II
_cod_database_code               2017271
_cod_database_fobs_code          2017271