#------------------------------------------------------------------------------
#$Date: 2019-12-26 21:19:10 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/17/2311727.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2311727
loop_
_publ_author_name
'Binns, Jack'
'McIntyre, Garry J.'
'Barreda-Argüeso, José A'
'González, Jesús'
'Aguado, Fernando'
'Rodríguez, Fernando'
'Valiente, Rafael'
'Parsons, Simon'
_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 H12 N1, Cl4 Ga1 '
_chemical_formula_sum            'C4 H12 Cl4 Ga N'
_chemical_formula_weight         285.68
_chemical_name_systematic        'tetramethylammonium tetrachlorogallate'
_space_group_IT_number           57
_space_group_name_Hall           '-P 2a 2ab'
_space_group_name_H-M_alt        'P b m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ab'
_symmetry_space_group_name_H-M   'P b m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-10-06
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8736(3)
_cell_length_b                   14.1743(3)
_cell_length_c                   6.4043(2)
_cell_measurement_reflns_used    3059
_cell_measurement_temperature    249
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     1168.62(5)
_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      249
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            15621
_diffrn_reflns_theta_full        25.344
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.212
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.18
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0000327
_refine_ls_shift/su_mean         0.0000327
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 8.42 13.0 7.19 2.51 0.458 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1055
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1055
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                1046
_reflns_number_total             1112
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0543
_oxford_refine_ls_scale          0.15440(8)
_oxford_reflns_number_all        1108
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'SP3084_248_Pbma in Pbma'
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           tcg_248
_cod_original_sg_symbol_H-M      'P b m a '
_cod_original_formula_sum        'C4 H12 Cl4 Ga1 N1'
_cod_database_code               2311727
_iucr_refine_instructions_details_constraints
;
#
# Punched on 06/10/15 at 11:56:42
#
#LIST     12                                                                    
FULL 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 06/10/15 at 11:56:42
#
#LIST     16                                                                    
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) 
VIBR .0, 0.00200 = N(1) TO C(2,4) 
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) TO C(1,4) 
VIBR .0, 0.00500 = C(1) TO C(1,4) 
VIBR .0, 0.00500 = C(1) TO C(2,4) 
VIBR .0, 0.00500 = C(2) TO C(1,4) 
VIBR .0, 0.00500 = C(2) TO C(2,4) 
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) 
U(IJ) .0, 0.04000 = N(1) TO C(2) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z
x+1/2,y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_adp
Ga1 Ga -0.0388 0.2500 0.1586 0.0355 1.0000 Uani .
Cl3 Cl 0.0219 0.3771 0.0186 0.0565 1.0000 Uani .
Cl2 Cl 0.0001 0.2500 0.4884 0.0655 1.0000 Uani .
Cl1 Cl -0.2067 0.2500 0.1255 0.0690 1.0000 Uani .
N1 N 0.2500 0.0000 0.4562 0.0396 1.0000 Uani U
C1 C 0.1608 0.0294 0.5842 0.1057 1.0000 Uani U
C2 C 0.2821 0.0803 0.3211 0.0961 1.0000 Uani U
H11 H 0.1052 0.0477 0.4956 0.1268 1.0000 Uiso .
H12 H 0.1803 0.0811 0.6698 0.1268 1.0000 Uiso .
H13 H 0.1393 -0.0218 0.6698 0.1268 1.0000 Uiso .
H21 H 0.3398 0.0618 0.2379 0.1154 1.0000 Uiso .
H22 H 0.3012 0.1324 0.4061 0.1154 1.0000 Uiso .
H23 H 0.2260 0.0978 0.2331 0.1154 1.0000 Uiso .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ga1 0.0405 0.0269 0.0389 0.0000 -0.0013 0.0000
Cl3 0.0690 0.0354 0.0650 0.0121 -0.0020 -0.0103
Cl2 0.0874 0.0708 0.0384 0.0000 -0.0071 0.0000
Cl1 0.0401 0.0693 0.0978 0.0000 -0.0021 0.0000
N1 0.0341 0.0353 0.0495 0.0000 0.0000 -0.0021
C1 0.1067 0.0918 0.1185 -0.0034 0.0636 0.0254
C2 0.0996 0.0929 0.0960 0.0454 -0.0037 -0.0355
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135
1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl3 5_555 Ga1 Cl3 . 113.124 yes
Cl3 5_555 Ga1 Cl2 . 108.717 yes
Cl3 . Ga1 Cl2 . 108.717 yes
Cl3 5_555 Ga1 Cl1 . 108.643 yes
Cl3 . Ga1 Cl1 . 108.643 yes
Cl2 . Ga1 Cl1 . 108.925 yes
C2 7_555 N1 C1 7_555 108.948 yes
C2 7_555 N1 C1 . 108.861 yes
C1 7_555 N1 C1 . 112.298 yes
C2 7_555 N1 C2 . 108.870 yes
C1 7_555 N1 C2 . 108.861 yes
C1 . N1 C2 . 108.948 yes
N1 . C1 H11 . 109.5 no
N1 . C1 H12 . 109.5 no
H11 . C1 H12 . 109.5 no
N1 . C1 H13 . 109.5 no
H11 . C1 H13 . 109.5 no
H12 . C1 H13 . 109.5 no
N1 . C2 H21 . 109.5 no
N1 . C2 H22 . 109.5 no
H21 . C2 H22 . 109.5 no
N1 . C2 H23 . 109.5 no
H21 . C2 H23 . 109.5 no
H22 . C2 H23 . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ga1 Cl3 5_555 2.158 yes
Ga1 Cl3 . 2.158 yes
Ga1 Cl2 . 2.17073(6) yes
Ga1 Cl1 . 2.17164(5) yes
N1 C2 7_555 1.488 yes
N1 C1 7_555 1.471 yes
N1 C1 . 1.471 yes
N1 C2 . 1.488 yes
C1 H11 . 0.950 no
C1 H12 . 0.950 no
C1 H13 . 0.950 no
C2 H21 . 0.950 no
C2 H22 . 0.950 no
C2 H23 . 0.950 no
