Phase transition sequences in tetramethylammonium tetrachlorometallates by X-ray diffraction and spectroscopic measurements.
Binns, Jack; McIntyre, Garry J.; Barreda-Argüeso, José A; González, Jesús; Aguado, Fernando; Rodríguez, Fernando; Valiente, Rafael; Parsons, Simon; Acta crystallographica Section B, Structural science, crystal engineering and materials 73 (2017) 844–855; doi:10.1107/S2052520617006412

data_2311729
_publ_section_title
;
 Phase transition sequences in tetramethylammonium tetrachlorometallates
 by X-ray diffraction and spectroscopic measurements.
;
_journal_issue                   'Pt 5'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              844
_journal_page_last               855
_journal_paper_doi               10.1107/S2052520617006412
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C4 Cl4 Ga1 N1'
_chemical_formula_sum            'C4 Cl4 Ga N'
_chemical_formula_weight         273.58
_chemical_name_systematic        'Tetramethylammonium tetrachlorogallate(III)'
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-11-26
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.8504(4)
_cell_length_b                   6.8504(4)
_cell_length_c                   6.8504(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    393
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.8
_cell_volume                     321.48(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      393
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1506
_diffrn_reflns_theta_full        15.638
_diffrn_reflns_theta_max         15.638
_diffrn_reflns_theta_min         2.974
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.917
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             130
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9988
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         29
_refine_ls_number_restraints     86
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.0000059
_refine_ls_shift/su_mean         0.0000015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1549
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1549
_reflns_limit_h_max              3
_reflns_limit_h_min              0
_reflns_limit_k_max              3
_reflns_limit_k_min              0
_reflns_limit_l_max              5
_reflns_limit_l_min              1
_reflns_number_gt                29
_reflns_number_total             30
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0951
_oxford_refine_ls_scale          2.5(2)
_oxford_reflns_number_all        29
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'TCG in Pm-3m'
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           tcg_393
_cod_original_sg_symbol_H-M      'P m -3 m '
_cod_original_formula_sum        'C4 Cl4 Ga1 N1'
_cod_database_code               2311729
_iucr_refine_instructions_details_constraints
;
FULL GA(1,X'S,U'S) UNTIL N(4) C(100,U[ISO],SIZE) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = GA(1) TO CL(3,-9) 
VIBR .0, 0.00200 = GA(1) TO CL(3,4) 
VIBR .0, 0.00200 = GA(1) TO CL(3,-4) 
VIBR .0, 0.00200 = GA(1) TO CL(3,7) 
VIBR .0, 0.00200 = GA(1) TO CL(3,-7) 
VIBR .0, 0.00200 = GA(1) TO CL(3,9) 
VIBR .0, 0.00200 = GA(1) TO CL(3) 
VIBR .0, 0.00200 = GA(1) TO CL(2) 
VIBR .0, 0.00500 = CL(3,4) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3,-4) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3,-4) TO CL(3,4) 
VIBR .0, 0.00500 = CL(3,7) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3,7) TO CL(3,4) 
VIBR .0, 0.00500 = CL(3,7) TO CL(3,-4) 
VIBR .0, 0.00500 = CL(3,-7) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3,-7) TO CL(3,4) 
VIBR .0, 0.00500 = CL(3,-7) TO CL(3,-4) 
VIBR .0, 0.00500 = CL(3,-7) TO CL(3,7) 
VIBR .0, 0.00500 = CL(3,9) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3,9) TO CL(3,4) 
VIBR .0, 0.00500 = CL(3,9) TO CL(3,-4) 
VIBR .0, 0.00500 = CL(3,9) TO CL(3,7) 
VIBR .0, 0.00500 = CL(3,9) TO CL(3,-7) 
VIBR .0, 0.00500 = CL(3) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(3) TO CL(3,4) 
VIBR .0, 0.00500 = CL(3) TO CL(3,-4) 
VIBR .0, 0.00500 = CL(3) TO CL(3,7) 
VIBR .0, 0.00500 = CL(3) TO CL(3,-7) 
VIBR .0, 0.00500 = CL(3) TO CL(3,9) 
VIBR .0, 0.00500 = CL(2) TO CL(3,-9) 
VIBR .0, 0.00500 = CL(2) TO CL(3,4) 
VIBR .0, 0.00500 = CL(2) TO CL(3,-4) 
VIBR .0, 0.00500 = CL(2) TO CL(3,7) 
VIBR .0, 0.00500 = CL(2) TO CL(3,-7) 
VIBR .0, 0.00500 = CL(2) TO CL(3,9) 
VIBR .0, 0.00500 = CL(2) TO CL(3) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,-9) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,4) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,-4) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,7) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,-7) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3,9) 
U(IJ) .0, 0.04000 = GA(1) TO CL(3) 
U(IJ) .0, 0.08000 = GA(1) TO CL(2) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.200000 , 0.050000 = GA(1) TO CL(3) 
DISTANCE 2.200000 , 0.050000 = GA(1) TO CL(2) 
END                                                                             
;