#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/57/1505742.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1505742
loop_
_publ_author_name
'Bujak, Maciej'
'Angel, Ross J.'
_publ_section_title
;
 High-pressure- and low-temperature-induced changes in
 [(CH3)2NH(CH2)2NH3][SbCl5].
;
_journal_issue                   21
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              10322
_journal_page_last               10331
_journal_paper_doi               10.1021/jp060652v
_journal_volume                  110
_journal_year                    2006
_chemical_formula_moiety         '2(C4 H14 N2), Cl6 Sb, Cl4 Sb'
_chemical_formula_sum            'C8 H28 Cl10 N4 Sb2'
_chemical_formula_weight         778.34
_chemical_name_common
; 
  N,N-Dimethylethylenediammonium Pentachloroantimonate(III)   
;
_chemical_name_systematic
; 
  N,N-Dimethylethylenediammonium Pentachloroantimonate(III)   
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.171(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0842(16)
_cell_length_b                   9.7970(6)
_cell_length_c                   9.7670(4)
_cell_measurement_pressure       3100000
_cell_measurement_reflns_used    27
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      12.8
_cell_measurement_theta_min      4.4
_cell_volume                     2201.8(2)
_computing_cell_refinement
;
 Single software; Angel, R. J.; Downs, R. T.; Finger, L. W. High-Pressure and 
 High-Temperature Crystal Chemistry; edited by R. M. Hazen and R. T. Downs, 
 pp. 559 - 596. The Mineralogical  Society of America: Washington DC, 2000 
;
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2004)'
_computing_data_reduction
; 
 CrysAlis RED (Oxford Diffraction, 2004); AVERAGE v2.2 (R. J. Angel, 2003), 
 www. crystal.vt.edu 
;
_computing_molecular_graphics    'Bruker SHELXTL NT (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      'Diamond-anvil cell, N~2~ pressure medium'
_diffrn_ambient_pressure         3100000
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.368
_diffrn_measured_fraction_theta_max 0.368
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-1'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.0952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1422
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_T_max  0.7578
_exptl_absorpt_correction_T_min  0.4728
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
  Correction for absorption affects of the diamond anvil cell
  and the sample were made using ABSORB 6.0;  
  R. J. Angel, J. Appl. Cryst. (2004) 37, 486
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1422
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                888
_reflns_number_total             1422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp060652vsi20060131_042319.cif
_cod_data_source_block           3.10GPa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1505742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sb11 Sb 0.11425(13) 0.96881(10) 0.29885(14) 0.0180(15) Uani 1 1 d U
Cl11 Cl 0.1707(5) 1.0727(4) 0.1636(5) 0.029(3) Uani 1 1 d U
Cl12 Cl 0.0454(5) 1.1512(4) 0.2416(5) 0.032(3) Uani 1 1 d U
Cl13 Cl 0.2061(4) 0.7586(4) 0.3669(5) 0.023(3) Uani 1 1 d U
Cl14 Cl 0.0618(5) 0.8397(4) 0.0692(5) 0.032(3) Uani 1 1 d U
Cl15 Cl 0.1750(4) 1.1225(4) 0.5054(5) 0.023(3) Uani 1 1 d U
Sb21 Sb 0.11131(13) 0.78588(10) 0.79311(13) 0.0213(15) Uani 1 1 d U
Cl21 Cl 0.1770(5) 0.6883(4) 0.6800(5) 0.023(3) Uani 1 1 d U
Cl22 Cl 0.0455(5) 0.5948(4) 0.6973(5) 0.034(3) Uani 1 1 d U
Cl23 Cl 0.1984(5) 0.9894(4) 0.8577(5) 0.021(3) Uani 1 1 d U
Cl24 Cl 0.0671(5) 0.9130(4) 0.5592(5) 0.025(3) Uani 1 1 d U
Cl25 Cl 0.1640(4) 0.6249(4) 1.0030(5) 0.022(3) Uani 1 1 d U
N11 N 0.2412(14) 0.3306(12) 0.3626(16) 0.027(3) Uani 1 1 d U
H111 H 0.2665 0.3096 0.3154 0.032 Uiso 1 1 d R
H112 H 0.2584 0.3839 0.4369 0.032 Uiso 1 1 d R
H113 H 0.2289 0.2545 0.3940 0.032 Uiso 1 1 d R
C11 C 0.1912(17) 0.4110(16) 0.2646(18) 0.021(3) Uani 1 1 d U
H114 H 0.1734 0.3550 0.1813 0.025 Uiso 1 1 d R
H115 H 0.2055 0.4933 0.2314 0.025 Uiso 1 1 d R
C12 C 0.1407(16) 0.4513(15) 0.3355(18) 0.017(3) Uani 1 1 d U
H116 H 0.1192 0.3704 0.3465 0.021 Uiso 1 1 d R
H117 H 0.1594 0.4876 0.4303 0.021 Uiso 1 1 d R
N12 N 0.1030(13) 0.5508(12) 0.2551(15) 0.025(3) Uani 1 1 d U
H118 H 0.1232 0.6178 0.2263 0.029 Uiso 1 1 d R
C13 C 0.0624(18) 0.4827(16) 0.1283(17) 0.030(4) Uani 1 1 d U
H119 H 0.0836 0.4429 0.0690 0.046 Uiso 1 1 d R
H120 H 0.0411 0.4126 0.1600 0.046 Uiso 1 1 d R
H121 H 0.0357 0.5497 0.0742 0.046 Uiso 1 1 d R
C14 C 0.0711(16) 0.6103(15) 0.3498(19) 0.028(4) Uani 1 1 d U
H122 H 0.0973 0.6534 0.4320 0.042 Uiso 1 1 d R
H123 H 0.0445 0.6768 0.2949 0.042 Uiso 1 1 d R
H124 H 0.0498 0.5397 0.3807 0.042 Uiso 1 1 d R
N21 N 0.2267(13) 0.4214(12) 0.8556(15) 0.022(3) Uani 1 1 d U
H211 H 0.2534 0.4486 0.8148 0.026 Uiso 1 1 d R
H212 H 0.2436 0.3704 0.9320 0.026 Uiso 1 1 d R
H213 H 0.2104 0.4941 0.8826 0.026 Uiso 1 1 d R
C21 C 0.1864(17) 0.3427(16) 0.7627(18) 0.023(3) Uani 1 1 d U
H214 H 0.1695 0.3953 0.6763 0.027 Uiso 1 1 d R
H215 H 0.2045 0.2624 0.7362 0.027 Uiso 1 1 d R
C22 C 0.1356(16) 0.2955(15) 0.8265(17) 0.015(3) Uani 1 1 d U
H216 H 0.1132 0.3748 0.8378 0.018 Uiso 1 1 d R
H217 H 0.1529 0.2562 0.9206 0.018 Uiso 1 1 d R
N22 N 0.0985(13) 0.2005(12) 0.7415(15) 0.022(3) Uani 1 1 d U
H218 H 0.1198 0.1311 0.7206 0.027 Uiso 1 1 d R
C23 C 0.0619(17) 0.2610(15) 0.6043(19) 0.025(4) Uani 1 1 d U
H219 H 0.0896 0.2928 0.5583 0.038 Uiso 1 1 d R
H220 H 0.0397 0.3368 0.6219 0.038 Uiso 1 1 d R
H221 H 0.0363 0.1961 0.5435 0.038 Uiso 1 1 d R
C24 C 0.0602(15) 0.1470(15) 0.8194(18) 0.028(4) Uani 1 1 d U
H222 H 0.0824 0.1020 0.9055 0.042 Uiso 1 1 d R
H223 H 0.0334 0.0834 0.7599 0.042 Uiso 1 1 d R
H224 H 0.0391 0.2217 0.8437 0.042 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
Cl11 Sb11 Cl12 91.2(3) .
Cl11 Sb11 Cl13 84.9(2) .
Cl11 Sb11 Cl14 86.6(2) .
Cl11 Sb11 Cl15 84.3(2) .
Cl12 Sb11 Cl13 175.6(3) .
Cl12 Sb11 Cl14 92.0(2) .
Cl12 Sb11 Cl15 86.6(3) .
Cl14 Sb11 Cl13 89.8(2) .
Cl15 Sb11 Cl13 91.0(2) .
Cl14 Sb11 Cl15 170.74(18) .
Cl11 Sb11 Cl24 158.3(2) .
Cl12 Sb11 Cl24 85.83(19) .
Cl13 Sb11 Cl24 97.07(17) .
Cl14 Sb11 Cl24 115.0(2) .
Cl15 Sb11 Cl24 74.1(2) .
Sb11 Cl14 Sb21 126.3(3) 1_554
Cl21 Sb21 Cl22 87.7(3) .
Cl21 Sb21 Cl23 80.5(2) .
Cl21 Sb21 Cl24 86.5(2) .
Cl21 Sb21 Cl25 83.5(2) .
Cl22 Sb21 Cl23 167.6(2) .
Cl22 Sb21 Cl24 88.8(2) .
Cl22 Sb21 Cl25 87.0(2) .
Cl24 Sb21 Cl23 86.7(2) .
Cl25 Sb21 Cl23 95.4(2) .
Cl24 Sb21 Cl25 169.29(17) .
Cl21 Sb21 Cl14 153.4(2) 1_556
Cl22 Sb21 Cl14 94.9(2) 1_556
Cl23 Sb21 Cl14 97.37(17) 1_556
Cl24 Sb21 Cl14 120.0(2) 1_556
Cl25 Sb21 Cl14 70.24(19) 1_556
Sb21 Cl24 Sb11 131.3(4) .
C11 N11 H111 109.3 .
C11 N11 H112 107.5 .
H111 N11 H112 109.5 .
C11 N11 H113 111.6 .
H111 N11 H113 109.5 .
H112 N11 H113 109.5 .
N11 C11 C12 114.4(13) .
N11 C11 H114 107.9 .
C12 C11 H114 107.1 .
N11 C11 H115 110.3 .
C12 C11 H115 109.1 .
H114 C11 H115 107.6 .
N12 C12 C11 112.0(13) .
N12 C12 H116 110.6 .
C11 C12 H116 109.9 .
N12 C12 H117 108.7 .
C11 C12 H117 107.5 .
H116 C12 H117 107.9 .
C12 N12 C14 107.0(14) .
C12 N12 C13 108.1(14) .
C14 N12 C13 111(3) .
C12 N12 H118 110.9 .
C14 N12 H118 109.4 .
C13 N12 H118 110.2 .
N12 C13 H119 110.3 .
N12 C13 H120 109.5 .
H119 C13 H120 109.5 .
N12 C13 H121 108.6 .
H119 C13 H121 109.5 .
H120 C13 H121 109.5 .
N12 C14 H122 111.2 .
N12 C14 H123 107.6 .
H122 C14 H123 109.5 .
N12 C14 H124 109.6 .
H122 C14 H124 109.5 .
H123 C14 H124 109.5 .
C21 N21 H211 109.8 .
C21 N21 H212 107.5 .
H211 N21 H212 109.5 .
C21 N21 H213 111.1 .
H211 N21 H213 109.5 .
H212 N21 H213 109.5 .
N21 C21 C22 112.5(14) .
N21 C21 H214 108.3 .
C22 C21 H214 108.6 .
N21 C21 H215 110.5 .
C22 C21 H215 108.9 .
H214 C21 H215 107.8 .
N22 C22 C21 113.2(14) .
N22 C22 H216 109.0 .
C21 C22 H216 109.1 .
N22 C22 H217 108.8 .
C21 C22 H217 108.7 .
H216 C22 H217 107.9 .
C22 N22 C24 109.0(14) .
C22 N22 C23 112.1(13) .
C24 N22 C23 108(3) .
C22 N22 H218 109.2 .
C24 N22 H218 109.6 .
C23 N22 H218 108.5 .
N22 C23 H219 104.0 .
N22 C23 H220 111.1 .
H219 C23 H220 109.5 .
N22 C23 H221 113.2 .
H219 C23 H221 109.5 .
H220 C23 H221 109.5 .
N22 C24 H222 110.3 .
N22 C24 H223 109.5 .
H222 C24 H223 109.5 .
N22 C24 H224 108.6 .
H222 C24 H224 109.5 .
H223 C24 H224 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb11 Cl11 2.386(7) .
Sb11 Cl12 2.389(8) .
Sb11 Cl13 2.950(8) .
Sb11 Cl14 2.560(6) .
Sb11 Cl15 2.595(6) .
Sb11 Cl24 3.124(5) .
Sb21 Cl21 2.381(7) .
Sb21 Cl22 2.454(8) .
Sb21 Cl23 2.827(8) .
Sb21 Cl24 2.544(6) .
Sb21 Cl25 2.601(6) .
Sb21 Cl14 3.297(5) 1_556
N11 C11 1.52(4) .
N11 H111 0.8902 .
N11 H112 0.8900 .
N11 H113 0.8899 .
C11 C12 1.62(4) .
C11 H114 0.9700 .
C11 H115 0.9700 .
C12 N12 1.40(3) .
C12 H116 0.9700 .
C12 H117 0.9700 .
N12 C14 1.48(2) .
N12 C13 1.49(3) .
N12 H118 0.9100 .
C13 H119 0.9598 .
C13 H120 0.9601 .
C13 H121 0.9600 .
C14 H122 0.9600 .
C14 H123 0.9599 .
C14 H124 0.9600 .
N21 C21 1.36(4) .
N21 H211 0.8899 .
N21 H212 0.8900 .
N21 H213 0.8900 .
C21 C22 1.60(4) .
C21 H214 0.9700 .
C21 H215 0.9700 .
C22 N22 1.38(3) .
C22 H216 0.9700 .
C22 H217 0.9700 .
N22 C24 1.46(3) .
N22 C23 1.49(3) .
N22 H218 0.9100 .
C23 H219 0.9600 .
C23 H220 0.9600 .
C23 H221 0.9599 .
C24 H222 0.9600 .
C24 H223 0.9599 .
C24 H224 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H111 Cl13 0.89 2.13 2.969(18) 156.1 2_545
N11 H111 Cl25 0.89 2.73 3.04(3) 101.5 2_546
N11 H112 Cl23 0.89 2.22 3.106(19) 171.4 2_546
N11 H113 Cl15 0.89 2.32 3.16(2) 156.7 1_545
N12 H118 Cl13 0.91 2.48 3.15(3) 130.2 .
N12 H118 Cl25 0.91 2.64 3.298(17) 129.6 1_554
N21 H211 Cl15 0.89 2.68 3.07(2) 107.9 2_546
N21 H211 Cl23 0.89 2.35 3.20(2) 161.4 2_546
N21 H212 Cl13 0.89 2.26 3.15(2) 173.7 2_546
N21 H213 Cl21 0.89 2.69 3.162(17) 114.2 .
N21 H213 Cl25 0.89 2.25 3.102(18) 160.5 .
N22 H218 Cl23 0.91 2.41 3.12(3) 135.1 1_545
N22 H218 Cl24 0.91 2.74 3.298(14) 121.0 1_545
C11 H114 Cl11 0.97 2.77 3.451(17) 127.8 1_545
C11 H115 Cl25 0.97 2.51 3.218(16) 129.4 1_554
C14 H124 Cl22 0.96 2.56 3.37(3) 142.3 3_566
C21 H215 Cl15 0.97 2.55 3.261(15) 129.8 1_545
C23 H219 Cl15 0.96 2.81 3.43(3) 122.7 1_545
C23 H220 Cl22 0.96 2.62 3.447(16) 144.0 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cl11 Sb11 Cl14 Sb21 20.8(3) . 1_554
Cl12 Sb11 Cl14 Sb21 111.9(3) . 1_554
Cl13 Sb11 Cl14 Sb21 -64.1(3) . 1_554
Cl15 Sb11 Cl14 Sb21 30.4(18) . 1_554
Cl11 Sb11 Cl24 Sb21 -76.9(7) . .
Cl12 Sb11 Cl24 Sb21 -159.6(3) . .
Cl13 Sb11 Cl24 Sb21 17.0(3) . .
Cl14 Sb11 Cl24 Sb21 110.1(3) . .
Cl15 Sb11 Cl24 Sb21 -72.0(3) . .
Cl24 Sb11 Cl14 Sb21 -161.7(2) . 1_554
Cl14 Sb21 Cl24 Sb11 160.7(2) 1_556 .
Cl21 Sb21 Cl24 Sb11 -16.6(3) . .
Cl22 Sb21 Cl24 Sb11 -104.4(3) . .
Cl23 Sb21 Cl24 Sb11 64.1(3) . .
Cl25 Sb21 Cl24 Sb11 -37.5(18) . .
N11 C11 C12 N12 166(2) . .
C11 C12 N12 C13 78(3) . .
C11 C12 N12 C14 -162.7(19) . .
N21 C21 C22 N22 -172(2) . .
C21 C22 N22 C23 -70(3) . .
C21 C22 N22 C24 170(2) . .
