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_2311723
_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 Fe1 N1'
_chemical_formula_sum            'C4 Cl4 Fe N'
_chemical_formula_weight         259.71
_chemical_name_systematic        'tetramethylammonium tetrachloroferrate(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             15-07-08
_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                   6.8470(5)
_cell_length_b                   6.8470(5)
_cell_length_c                   6.8470(5)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    365
_cell_measurement_theta_max      28.5219
_cell_measurement_theta_min      2.9706
_cell_volume                     321.00(4)
_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      365
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details
;
  1 omega  -14.00   79.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436   77.0000   90.0000 93

  2 omega  -16.00   74.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436   38.0000    0.0000 90

  3 omega  -18.00   82.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436   57.0000 -120.0000 100

  4 omega  -16.00   52.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -99.0000   60.0000 68

  5 omega  -41.00   44.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -77.0000  -60.0000 85

  6 omega   32.00   67.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436 -124.0000 -125.0000 35

  7 omega  -63.00   13.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -38.0000 -180.0000 76

  8 omega   13.00   60.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436 -112.0000  110.0898 47

  9 omega  -88.00   25.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       -8.9155  -77.0000  -60.0000 113

 10 omega  -20.00   33.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       -8.9155  -99.0000  150.0000 53

 11 omega  -64.00   40.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -57.0000   60.0000 104

 12 omega  -20.00   52.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -99.0000  -90.0000 72

 13 omega  -68.00   44.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -77.0000    0.0000 112

 14 omega  -20.00   52.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436  -99.0000 -180.0000 72

 15 omega    1.00   64.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436 -124.0000 -125.0000 63

 16 omega   -9.00   60.00   1.0000    2.6100
omega____ theta____ kappa____ phi______ frames
    -       10.2436 -112.0000  110.0898 69

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0102712000
_diffrn_orient_matrix_UB_12      -0.1025522000
_diffrn_orient_matrix_UB_13      -0.0108929000
_diffrn_orient_matrix_UB_21      0.1028035000
_diffrn_orient_matrix_UB_22      -0.0094600000
_diffrn_orient_matrix_UB_23      -0.0082067000
_diffrn_orient_matrix_UB_31      0.0071652000
_diffrn_orient_matrix_UB_32      -0.0116587000
_diffrn_orient_matrix_UB_33      0.1026661000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1895
_diffrn_reflns_theta_full        13.6761
_diffrn_reflns_theta_max         13.3936
_diffrn_reflns_theta_min         2.9690
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             125
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9907
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         18
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.0000156
_refine_ls_shift/su_mean         0.0000040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 13.8 13.1 9.98 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1380
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1380
_reflns_limit_h_max              2
_reflns_limit_h_min              0
_reflns_limit_k_max              3
_reflns_limit_k_min              0
_reflns_limit_l_max              4
_reflns_limit_l_min              1
_reflns_number_gt                18
_reflns_number_total             21
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   14.74
_oxford_diffrn_Wilson_scale      0.89
_oxford_refine_ls_r_factor_ref   0.0981
_oxford_refine_ls_scale          2.7(2)
_oxford_reflns_number_all        18
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'TCF in Pm-3m'
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           tcf_cP22
_cod_original_cell_volume        321.00(7)
_cod_original_sg_symbol_H-M      'P m -3 m '
_cod_original_formula_sum        'C4 Cl4 Fe1 N1'
_cod_database_code               2311723
_iucr_refine_instructions_details_constraints
;
FULL FE(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 = FE(1) TO CL(3,-9) 
VIBR .0, 0.00200 = FE(1) TO CL(3,4) 
VIBR .0, 0.00200 = FE(1) TO CL(3,-4) 
VIBR .0, 0.00200 = FE(1) TO CL(3,7) 
VIBR .0, 0.00200 = FE(1) TO CL(3,-7) 
VIBR .0, 0.00200 = FE(1) TO CL(3,9) 
VIBR .0, 0.00200 = FE(1) TO CL(3) 
VIBR .0, 0.00200 = FE(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 = FE(1) TO CL(3,-9) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3,4) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3,-4) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3,7) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3,-7) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3,9) 
U(IJ) .0, 0.04000 = FE(1) TO CL(3) 
U(IJ) .0, 0.08000 = FE(1) TO CL(2) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 2.200000 , 0.050000 = FE(1) TO CL(3) 
DISTANCE 2.200000 , 0.050000 = FE(1) TO CL(2) 
END                                                                             
;