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#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/14/2101489.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_2101489
loop_
_publ_author_name
'Zaleski, J.'
'Pietraszko, A.'
_publ_section_title
;
 Structure at 200 and 298 K and X-ray investigations of the phase
 transition at 242 K of [NH₂(CH₃)₂]₃Sb₂Cl₉ (DMACA)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              287
_journal_page_last               295
_journal_paper_doi               10.1107/S0108768195010615
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C6 H24 Cl9 N3 Sb2'
_chemical_formula_weight         700.8
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 95.81(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   9.470(3)
_cell_length_b                   9.034(3)
_cell_length_c                   14.080(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    200
_cell_measurement_theta_max      15
_cell_measurement_theta_min      9.5
_cell_volume                     1198.4(6)
_diffrn_measurement_device       'Kuma KM-4'
_diffrn_measurement_method       ω-θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10529
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.28
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.50
_refine_ls_goodness_of_fit_obs   0.95
_refine_ls_hydrogen_treatment
;H atoms were placed in calculated positions; methyl H atoms
were not refined, positional and displacement parameters for
all others were refined
;
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4613
_refine_ls_R_factor_obs          0.0241
_refine_ls_structure_factor_coef F
_refine_ls_wR_factor_obs         0.0252
_reflns_number_observed          4613
_reflns_number_total             5788
_reflns_observed_criterion       F>4.0\s(F)
_cod_data_source_file            hr0024.cif
_cod_data_source_block           hr0024a
_cod_original_cell_volume        1198.4(4)
_cod_database_code               2101489
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Sb(1) .0 .2102 .0 .0260(10)
Sb(2) .32450(10) .70430(10) .16870(10) .0250(10)
Cl(1) .4541(2) .5329(2) .27580(10) .0410(10)
Cl(2) -.1457(2) .0217(2) -.0809(2) .0480(10)
Cl(3) -.1830(2) .3923(2) -.0523(2) .0410(10)
Cl(4) .1925(2) -.0347(2) .04900(10) .0450(10)
Cl(5) .4571(2) .6554(2) .03630(10) .0410(10)
Cl(6) -.1279(2) .1663(2) .15140(10) .0420(10)
Cl(7) .5227(2) .8972(2) .2224(2) .0430(10)
Cl(8) .1564(2) .4853(2) .10830(10) .0440(10)
Cl(9) .1149(2) .7617(2) .33380(10) .0550(10)
N(1) .1176(6) -.1802(6) -.1609(4) .0500(10)
C(1) .2500(9) -.1669(10) -.2038(7) .0560(10)
C(2) .0843(11) -.3316(11) -.1334(7) .072(2)
N(2) -.1885(6) .6973(6) .2069(4) .0460(10)
C(3) -.2025(6) .5350(7) .1969(4) .0410(10)
C(4) -.1546(8) .7672(8) .1180(7) .0630(10)
N(31) .5327(8) .8726(8) .5520(5) .0450(10)
C(51) .4944(12) .7374(12) .6007(11) .081(2)
C(61) .5021(11) .8871(16) .4493(7) .072(2)
N(32) .483(3) .819(2) .473(2) .094(2)
C(52) .454(3) .721(3) .543(2) .083(2)
C(62) .542(3) .972(2) .496(2) .100(2)
H(1A) .046(3) -.137(3) -.208(3) .060
H(1B) .135(3) -.125(3) -.115(3) .060
H(2A) -.113(3) .734(3) .247(3) .060
H(2B) -.274(3) .743(3) .211(3) .060
H(31A) .635(3) .885(3) .568(3) .060
H(31B) .495(3) .935(3) .583(3) .060
H(32A) .406(3) .819(3) .442(3) .100
H(32B) .559(3) .772(3) .452(3) .100
H(1C) .2667 -.0659 -.2206 .080
H(1D) .3262 -.2007 -.1588 .080
H(1E) .2451 -.2275 -.2601 .080
H(2C) -.0043 -.3321 -.1058 .080
H(2D) .0772 -.3943 -.1887 .080
H(2E) .1582 -.3676 -.0875 .080
H(3A) -.2254 .4928 .2561 .080
H(3B) -.2766 .5123 .1474 .080
H(3C) -.1144 .4945 .1806 .080
H(4A) -.1466 .8723 .1270 .080
H(4B) -.0661 .7285 .1011 .080
H(4C) -.2283 .7463 .0679 .080
H(51A) .5212 .7442 .6681 .080
H(51B) .3939 .7217 .5893 .080
H(51C) .5435 .6560 .5749 .080
H(61A) .5329 .9827 .4301 .080
H(61B) .5515 .8116 .4179 .080
H(61C) .4018 .8772 .4322 .080
H(52A) .4250 .6217 .5248 .080
H(52B) .5355 .7165 .5891 .080
H(52C) .3777 .7699 .5702 .080
H(62A) .5650 1.0228 .4396 .080
H(62B) .4667 1.0223 .5227 .080
H(62C) .6246 .9690 .5417 .080
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl(2) Sb(1) Cl(3) 88.80(10) yes
Cl(2) Sb(1) Cl(4) 83.70(10) yes
Cl(2) Sb(1) Cl(6) 89.30(10) yes
Cl(2) Sb(1) Cl(8) 172.50(10) yes
Cl(3) Sb(1) Cl(4) 172.50(10) yes
Cl(3) Sb(1) Cl(6) 88.60(10) yes
Cl(3) Sb(1) Cl(8) 84.30(10) yes
Cl(4) Sb(1) Cl(6) 91.20(10) yes
Cl(4) Sb(1) Cl(8) 103.20(10) yes
Cl(6) Sb(1) Cl(8) 87.70(10) yes
Cl(1) Sb(2) Cl(5) 95.50(10) yes
Cl(1) Sb(2) Cl(7) 86.60(10) yes
Cl(1) Sb(2) Cl(8) 88.40(10) yes
Cl(1) Sb(2) Cl(9) 87.90(10) yes
Cl(5) Sb(2) Cl(7) 86.00(10) yes
Cl(5) Sb(2) Cl(8) 87.60(10) yes
Cl(5) Sb(2) Cl(9) 174.00(10) yes
Cl(7) Sb(2) Cl(8) 171.40(10) yes
Cl(7) Sb(2) Cl(9) 99.20(10) yes
Cl(8) Sb(2) Cl(9) 87.60(10) yes
Sb(1) Cl(8) Sb(2) 167.30(10) yes
C(1) N(1) C(2) 114.0(10) yes
C(3) N(2) C(4) 112.0(10) yes
C(51) N(31) C(61) 121.0(10) yes
C(52) N(32) C(62) 122(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sb(1) Cl(2) 2.405(2) yes
Sb(1) Cl(3) 2.447(2) yes
Sb(1) Cl(4) 2.905(2) yes
Sb(1) Cl(6) 2.587(2) yes
Sb(1) Cl(8) 3.199(2) yes
Sb(2) Cl(1) 2.409(2) yes
Sb(2) Cl(5) 2.393(2) yes
Sb(2) Cl(7) 2.617(2) yes
Sb(2) Cl(8) 2.625(2) yes
Sb(2) Cl(9) 3.247(2) yes
N(1) C(1) 1.450(10) yes
N(1) C(2) 1.460(10) yes
N(2) C(3) 1.480(10) yes
N(2) C(4) 1.470(10) yes
N(31) C(51) 1.460(10) yes
N(31) C(61) 1.450(10) yes
N(32) C(52) 1.37(4) yes
N(32) C(62) 1.52(3) yes
