#------------------------------------------------------------------------------
#$Date: 2016-04-05 18:31:24 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181616 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/43/7224386.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_7224386
loop_
_publ_author_name
'Wojtaś, Maciej'
'Bil, Andrzej'
'Ga̧gor, Anna'
'Medycki, Wojciech'
'Kholkin, Andrei L.'
_publ_section_title
;
 Phase stability and dynamics of hybrid organic--inorganic crystals
 [(CH3)3PH][SbCl4] and [(CH3)3PH][SbBr4]: a computational and NMR approach
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2413
_journal_paper_doi               10.1039/C6CE00160B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C6 H20 Cl8 P2 Sb2'
_chemical_formula_weight         681.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-04-23 deposited with the CCDC.
2016-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.283(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7270(7)
_cell_length_b                   31.123(2)
_cell_length_c                   9.4423(9)
_cell_measurement_reflns_used    8452
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.5245
_cell_measurement_theta_min      2.9145
_cell_volume                     2270.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21026
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    3.447
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.18 (release 25-02-2008 CrysAlis171 .NET)
(compiled Feb 25 2008,13:00:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.849
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.546
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.546
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0445
_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)+(0.0105P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                3606
_reflns_number_total             4306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00160b2.cif
_cod_data_source_block           1_295K
_cod_depositor_comments
'Adding full bibliography for 7224386--7224388.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7224386
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
Sb1 Sb 0.62648(4) 0.108772(10) 0.91090(4) 0.03766(9) Uani 1 1 d .
Sb2 Sb 0.12619(4) 0.134890(11) 0.75541(4) 0.03801(9) Uani 1 1 d .
Cl1 Cl 0.87057(18) 0.05622(4) 0.92826(16) 0.0521(4) Uani 1 1 d .
Cl2 Cl 0.4053(2) 0.05251(5) 0.91840(17) 0.0614(4) Uani 1 1 d .
Cl3 Cl 0.62739(18) 0.11123(4) 1.16407(14) 0.0492(4) Uani 1 1 d .
Cl4 Cl 0.37383(18) 0.17287(4) 0.93229(15) 0.0503(4) Uani 1 1 d .
Cl5 Cl 0.12453(18) 0.20159(4) 0.63175(15) 0.0488(4) Uani 1 1 d .
Cl6 Cl -0.10643(18) 0.10865(5) 0.58944(16) 0.0580(4) Uani 1 1 d .
Cl7 Cl 0.36315(19) 0.11148(5) 0.59159(16) 0.0576(4) Uani 1 1 d .
Cl8 Cl -0.11565(18) 0.17446(4) 0.93032(15) 0.0516(4) Uani 1 1 d .
P1 P 0.1350(2) 0.04445(5) 0.23420(16) 0.0486(4) Uani 1 1 d .
H1 H 0.146(7) 0.0340(18) 0.108(6) 0.073 Uiso 1 1 d .
C1 C 0.1344(7) 0.10145(17) 0.2310(6) 0.0529(16) Uani 1 1 d .
H1A H 0.1399 0.1122 0.3262 0.079 Uiso 1 1 calc R
H1B H 0.0301 0.1114 0.1862 0.079 Uiso 1 1 calc R
H1C H 0.2327 0.1115 0.1790 0.079 Uiso 1 1 calc R
C2 C -0.0597(8) 0.0238(2) 0.3050(7) 0.0656(19) Uani 1 1 d .
H2A H -0.0601 -0.0070 0.2965 0.098 Uiso 1 1 calc R
H2B H -0.1565 0.0355 0.2538 0.098 Uiso 1 1 calc R
H2C H -0.0680 0.0316 0.4031 0.098 Uiso 1 1 calc R
C3 C 0.3162(9) 0.0249(2) 0.3310(8) 0.080(2) Uani 1 1 d .
H3A H 0.4206 0.0318 0.2813 0.119 Uiso 1 1 calc R
H3B H 0.3071 -0.0057 0.3411 0.119 Uiso 1 1 calc R
H3C H 0.3188 0.0380 0.4231 0.119 Uiso 1 1 calc R
P11 P 0.12698(19) 0.30490(5) 0.92190(16) 0.0431(4) Uani 1 1 d .
H2 H 0.128(7) 0.3421(17) 0.918(6) 0.065 Uiso 1 1 d .
C11 C 0.1281(8) 0.2795(2) 1.0913(6) 0.0587(17) Uani 1 1 d .
H11A H 0.0264 0.2877 1.1426 0.088 Uiso 1 1 calc R
H11B H 0.2293 0.2882 1.1432 0.088 Uiso 1 1 calc R
H11C H 0.1291 0.2489 1.0791 0.088 Uiso 1 1 calc R
C21 C 0.3170(7) 0.29128(18) 0.8272(6) 0.0521(16) Uani 1 1 d .
H21A H 0.3242 0.2606 0.8176 0.078 Uiso 1 1 calc R
H21B H 0.4167 0.3016 0.8778 0.078 Uiso 1 1 calc R
H21C H 0.3130 0.3042 0.7350 0.078 Uiso 1 1 calc R
C31 C -0.0633(7) 0.29183(19) 0.8273(6) 0.0517(16) Uani 1 1 d .
H31A H -0.0512 0.3005 0.7303 0.077 Uiso 1 1 calc R
H31B H -0.1600 0.3065 0.8686 0.077 Uiso 1 1 calc R
H31C H -0.0822 0.2614 0.8314 0.077 Uiso 1 1 calc 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'
P P 0.1023 0.0942 '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
Cl3 Sb1 Cl2 89.57(5) .
Cl3 Sb1 Cl1 87.53(5) .
Cl2 Sb1 Cl1 93.25(5) .
Cl3 Sb1 Cl4 84.47(5) .
Cl2 Sb1 Cl4 91.17(5) .
Cl1 Sb1 Cl4 170.83(5) .
Cl3 Sb1 Cl8 85.09(5) 1_655
Cl2 Sb1 Cl8 174.66(5) 1_655
Cl1 Sb1 Cl8 86.46(4) 1_655
Cl4 Sb1 Cl8 88.39(4) 1_655
Cl5 Sb2 Cl7 87.31(5) .
Cl5 Sb2 Cl6 88.59(5) .
Cl7 Sb2 Cl6 92.47(5) .
Cl5 Sb2 Cl8 84.45(5) .
Cl7 Sb2 Cl8 170.57(5) .
Cl6 Sb2 Cl8 91.92(5) .
Cl5 Sb2 Cl4 85.78(5) .
Cl7 Sb2 Cl4 89.52(5) .
Cl6 Sb2 Cl4 173.94(5) .
Cl8 Sb2 Cl4 85.30(4) .
Sb2 Cl4 Sb1 97.54(4) .
Sb2 Cl8 Sb1 96.61(4) 1_455
C2 P1 C1 111.6(3) .
C2 P1 C3 110.5(3) .
C1 P1 C3 110.7(3) .
C2 P1 H1 109(3) .
C1 P1 H1 104(3) .
C3 P1 H1 110(3) .
P1 C1 H1A 109.5 .
P1 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
P1 C1 H1C 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
P1 C2 H2A 109.5 .
P1 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
P1 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
P1 C3 H3A 109.5 .
P1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
P1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C31 P11 C21 112.3(3) .
C31 P11 C11 110.6(3) .
C21 P11 C11 110.2(3) .
C31 P11 H2 103(3) .
C21 P11 H2 103(3) .
C11 P11 H2 118(3) .
P11 C11 H11A 109.5 .
P11 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
P11 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
P11 C21 H21A 109.5 .
P11 C21 H21B 109.5 .
H21A C21 H21B 109.5 .
P11 C21 H21C 109.5 .
H21A C21 H21C 109.5 .
H21B C21 H21C 109.5 .
P11 C31 H31A 109.5 .
P11 C31 H31B 109.5 .
H31A C31 H31B 109.5 .
P11 C31 H31C 109.5 .
H31A C31 H31C 109.5 .
H31B C31 H31C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Cl3 2.3917(14) .
Sb1 Cl2 2.4480(15) .
Sb1 Cl1 2.5012(14) .
Sb1 Cl4 2.7991(14) .
Sb1 Cl8 2.8601(14) 1_655
Sb2 Cl5 2.3818(14) .
Sb2 Cl7 2.5108(15) .
Sb2 Cl6 2.5150(14) .
Sb2 Cl8 2.7870(14) .
Sb2 Cl4 2.7958(14) .
P1 C2 1.771(6) .
P1 C1 1.774(5) .
P1 C3 1.776(7) .
P1 H1 1.24(6) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
P11 C31 1.764(5) .
P11 C21 1.774(6) .
P11 C11 1.784(6) .
P11 H2 1.16(5) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 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
C3 H3C Cl7 0.96 2.81 3.666(7) 149.5 .
P1 H1 Cl1 1.24(6) 2.83(5) 3.489(2) 112(3) 3_656
P1 H1 Cl1 1.24(6) 2.80(6) 3.549(2) 118(3) 1_454
P1 H1 Cl2 1.24(6) 2.76(6) 3.657(2) 128(3) 1_554
P11 H2 Cl3 1.16(5) 2.80(5) 3.569(2) 123(3) 4_565
