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_2311720
_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_absolute_configuration unk
_chemical_formula_moiety         'C4 H12 N1, Cl4 Fe1'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_chemical_name_systematic        'Tetramethylammonium tetrachloroferrate(III)'
_space_group_IT_number           28
_space_group_name_Hall           'P 2 -2b'
_space_group_name_H-M_alt        'P b m 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2b'
_symmetry_space_group_name_H-M   'P b m 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-09-23
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4471(5)
_cell_length_b                   14.2753(11)
_cell_length_c                   6.4526(5)
_cell_measurement_reflns_used    3355
_cell_measurement_temperature    295
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     593.86(8)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.042
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1248
_diffrn_reflns_theta_full        26.370
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.157
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9587
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1243
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.0018346
_refine_ls_shift/su_mean         0.0001393
_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: 
 16.3 25.1 12.7 3.20 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1301
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1301
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                1160
_reflns_number_total             1248
_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   0.0612
_oxford_refine_ls_scale          0.4101(15)
_oxford_reflns_number_all        1243
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title tcf_pbm2_295
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           TCF_oP44_295
_cod_original_sg_symbol_H-M      'P b m 2 '
_cod_original_formula_sum        'C4 H12 Cl4 Fe1 N1'
_cod_database_code               2311720
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
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 = N(1) TO C(1,4,1,2,1) 
VIBR .0, 0.00200 = N(1) TO C(2,4,1,2,1) 
VIBR .0, 0.00200 = N(1) TO C(1) 
VIBR .0, 0.00200 = N(1) TO C(2) 
VIBR .0, 0.00500 = C(2,4,1,2,1) TO C(1,4,1,2,1) 
VIBR .0, 0.00500 = C(1) TO C(1,4,1,2,1) 
VIBR .0, 0.00500 = C(1) TO C(2,4,1,2,1) 
VIBR .0, 0.00500 = C(2) TO C(1,4,1,2,1) 
VIBR .0, 0.00500 = C(2) TO C(2,4,1,2,1) 
VIBR .0, 0.00500 = C(2) TO C(1) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = N(1) TO C(1,4,1,2,1) 
U(IJ) .0, 0.04000 = N(1) TO C(2,4,1,2,1) 
U(IJ) .0, 0.04000 = N(1) TO C(1) 
U(IJ) .0, 0.04000 = N(1) TO C(2) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(1) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(2) 
ANGLE 109.500000 , 1.000000 = C(1) TO N(1) TO C(2) 
ANGLE 109.500000 , 1.000000 = C(1) TO N(1) TO C(2,4,1,1) 
ANGLE 109.500000 , 1.000000 = C(1) TO N(1) TO C(1,4,1,1) 
ANGLE 109.500000 , 1.000000 = C(2) TO N(1) TO C(1,4,1,1) 
ANGLE 109.500000 , 1.000000 = C(2) TO N(1) TO C(2,4,1,1) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(2) 
DISTANCE 1.450000 , 0.050000 = N(1) TO C(1) 
END                                                                             
;