#------------------------------------------------------------------------------
#$Date: 2019-12-26 21:19:10 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/17/2311724.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_2311724
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 2bc 2c'
_space_group_name_H-M_alt        'P c m b'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2c'
_symmetry_space_group_name_H-M   'P c m b'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-05-07
_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                   6.2820(4)
_cell_length_b                   14.0388(8)
_cell_length_c                   12.8067(8)
_cell_measurement_reflns_used    3159
_cell_measurement_temperature    100
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     1129.45(12)
_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      100
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.884
_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  0.035
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5262
_diffrn_reflns_theta_full        25.042
_diffrn_reflns_theta_max         28.784
_diffrn_reflns_theta_min         3.243
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.324
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.680
_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         2.24
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.0002203
_refine_ls_shift/su_mean         0.0000137
_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: 
 62.5 93.8 53.2 21.8 3.95 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1334
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1334
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1245
_reflns_number_total             1354
_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   0.0576
_oxford_refine_ls_scale          0.4613(16)
_oxford_reflns_number_all        1350
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'TCG in Pcmb at 100 K'
_cod_data_source_file            fx5008sup1.cif
_cod_data_source_block           tcg_100
_cod_original_sg_symbol_H-M      'P c m b '
_cod_original_formula_sum        'C4 H12 Cl4 Ga1 N1'
_cod_database_code               2311724
_iucr_refine_instructions_details_constraints
;
#
# Punched on 07/05/15 at 14:04:23
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  23,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   1,X'S) H   (  13,X'S) H   (  12,X'S) H   (  11,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 07/05/15 at 14:04:23
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y,z+1/2
x,-y,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x,-y+1/2,z+1/2
x,y+1/2,-z+1/2
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_posn
_atom_site_refinement_flags_adp
Ga1 Ga 0.32407(13) 0.2500 0.46375(6) 0.0138 1.0000 Uani S T
Cl2 Cl 0.4663(2) 0.37906(9) 0.52563(11) 0.0197 1.0000 Uani . .
Cl3 Cl -0.0134(3) 0.2500 0.50169(17) 0.0222 1.0000 Uani S T
Cl4 Cl 0.3614(3) 0.2500 0.29440(15) 0.0239 1.0000 Uani S T
N1 N -0.0467(10) 0.5000 0.2500 0.0133 1.0000 Uani S T
C2 C -0.1858(10) 0.4192(4) 0.2849(5) 0.0283 1.0000 Uani . .
C1 C 0.0868(11) 0.5318(5) 0.3392(5) 0.0303 1.0000 Uani . .
H23 H -0.0972 0.3654 0.3025 0.0423 1.0000 Uiso R .
H22 H -0.2672 0.4378 0.3451 0.0420 1.0000 Uiso R .
H21 H -0.2822 0.4023 0.2291 0.0421 1.0000 Uiso R .
H13 H 0.1706 0.5853 0.3188 0.0449 1.0000 Uiso R .
H12 H -0.0044 0.5480 0.3970 0.0450 1.0000 Uiso R .
H11 H 0.1760 0.4795 0.3595 0.0452 1.0000 Uiso R .
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 0.0161(4) 0.0091(4) 0.0163(4) 0.0000 0.0002(3) 0.0000
Cl2 0.0244(7) 0.0103(5) 0.0245(7) -0.0028(5) -0.0002(5) -0.0036(5)
Cl3 0.0161(9) 0.0204(9) 0.0300(10) 0.0000 0.0025(7) 0.0000
Cl4 0.0342(11) 0.0209(9) 0.0165(9) 0.0000 0.0014(8) 0.0000
N1 0.019(3) 0.007(3) 0.014(3) 0.002(2) 0.0000 0.0000
C2 0.030(3) 0.026(3) 0.029(3) 0.009(2) 0.000(3) -0.009(3)
C1 0.032(3) 0.027(3) 0.032(3) -0.001(3) -0.014(3) -0.002(3)
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
Cl2 5_555 Ga1 Cl2 . 113.21(8) yes
Cl2 5_555 Ga1 Cl3 . 108.65(5) yes
Cl2 . Ga1 Cl3 . 108.65(5) yes
Cl2 5_555 Ga1 Cl4 . 108.59(5) yes
Cl2 . Ga1 Cl4 . 108.59(5) yes
Cl3 . Ga1 Cl4 . 109.08(9) yes
C2 4_565 N1 C1 4_565 109.1(4) yes
C2 4_565 N1 C2 . 108.7(6) yes
C1 4_565 N1 C2 . 109.3(4) yes
C2 4_565 N1 C1 . 109.3(4) yes
C1 4_565 N1 C1 . 111.3(7) yes
C2 . N1 C1 . 109.1(4) yes
N1 . C2 H23 . 109.0 no
N1 . C2 H22 . 110.1 no
H23 . C2 H22 . 109.4 no
N1 . C2 H21 . 109.3 no
H23 . C2 H21 . 110.0 no
H22 . C2 H21 . 109.0 no
N1 . C1 H13 . 109.7 no
N1 . C1 H12 . 109.0 no
H13 . C1 H12 . 110.7 no
N1 . C1 H11 . 107.9 no
H13 . C1 H11 . 110.8 no
H12 . C1 H11 . 108.6 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 Cl2 5_555 2.1700(13) yes
Ga1 Cl2 . 2.1700(13) yes
Ga1 Cl3 . 2.175(2) yes
Ga1 Cl4 . 2.182(2) yes
N1 C2 4_565 1.500(7) yes
N1 C1 4_565 1.486(7) yes
N1 C2 . 1.500(7) yes
N1 C1 . 1.486(7) yes
C2 H23 . 0.965 no
C2 H22 . 0.961 no
C2 H21 . 0.966 no
C1 H13 . 0.953 no
C1 H12 . 0.964 no
C1 H11 . 0.960 no
