#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:14:32 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180174 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/70/7107065.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_7107065
loop_
_publ_author_name
'Saurabh S. Chitnis'
'Brendan Peters'
'Eamonn Conrad'
'Neil Burford'
'Robert McDonald'
'Michael J. Ferguson'
_publ_section_title
;
 Structural diversity for phosphine complexes of stibenium and
 stibinidenium cations
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              12331
_journal_paper_doi               10.1039/c1cc15693d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C26 H24 Cl2 P2 Sb, C H2 Cl2, Al Cl4'
_chemical_formula_sum            'C27 H26 Al Cl8 P2 Sb'
_chemical_formula_weight         844.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.3015(3)
_cell_angle_beta                 71.3838(3)
_cell_angle_gamma                87.5567(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5270(3)
_cell_length_b                   12.8155(3)
_cell_length_c                   14.0046(3)
_cell_measurement_reflns_used    9547
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.50
_cell_volume                     1721.72(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0142
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15558
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7930
_exptl_absorpt_correction_T_min  0.7060
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0252P)²+1.3868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                7215
_reflns_number_total             7895
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c1cc15693d.txt
_cod_data_source_block           dal1166
_cod_database_code               7107065
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sb Sb 0.338661(12) 0.034308(10) 0.435504(10) 0.02087(4) Uani 1 1 d .
Cl1 Cl 0.59898(5) -0.00045(4) 0.35470(4) 0.02557(10) Uani 1 1 d .
Cl2 Cl 0.12063(5) 0.12007(5) 0.46646(4) 0.03479(12) Uani 1 1 d .
P1 P 0.44784(5) 0.22577(4) 0.40123(4) 0.01958(10) Uani 1 1 d .
P2 P 0.35165(5) 0.11447(4) 0.23964(4) 0.02198(10) Uani 1 1 d .
C1 C 0.50035(19) 0.27858(16) 0.25920(15) 0.0240(4) Uani 1 1 d .
H1A H 0.5206 0.3577 0.2404 0.029 Uiso 1 1 calc R
H1B H 0.5841 0.2445 0.2285 0.029 Uiso 1 1 calc R
C2 C 0.3951(2) 0.25841(16) 0.21064(15) 0.0249(4) Uani 1 1 d .
H2A H 0.4303 0.2895 0.1338 0.030 Uiso 1 1 calc R
H2B H 0.3131 0.2963 0.2377 0.030 Uiso 1 1 calc R
C11 C 0.59456(19) 0.23458(15) 0.44016(15) 0.0224(4) Uani 1 1 d .
C12 C 0.7238(2) 0.22642(16) 0.37370(17) 0.0268(4) Uani 1 1 d .
H12 H 0.7357 0.2140 0.3076 0.032 Uiso 1 1 calc R
C13 C 0.8347(2) 0.23656(18) 0.40460(19) 0.0340(5) Uani 1 1 d .
H13 H 0.9223 0.2310 0.3595 0.041 Uiso 1 1 calc R
C14 C 0.8179(2) 0.25463(19) 0.5007(2) 0.0365(5) Uani 1 1 d .
H14 H 0.8940 0.2616 0.5214 0.044 Uiso 1 1 calc R
C15 C 0.6905(2) 0.26267(19) 0.56685(19) 0.0345(5) Uani 1 1 d .
H15 H 0.6794 0.2748 0.6330 0.041 Uiso 1 1 calc R
C16 C 0.5785(2) 0.25301(17) 0.53700(17) 0.0278(4) Uani 1 1 d .
H16 H 0.4912 0.2589 0.5825 0.033 Uiso 1 1 calc R
C21 C 0.32378(19) 0.30947(16) 0.46094(15) 0.0228(4) Uani 1 1 d .
C22 C 0.2503(2) 0.27105(18) 0.56706(16) 0.0280(4) Uani 1 1 d .
H22 H 0.2664 0.2018 0.6064 0.034 Uiso 1 1 calc R
C23 C 0.1539(2) 0.3340(2) 0.61481(19) 0.0365(5) Uani 1 1 d .
H23 H 0.1045 0.3084 0.6872 0.044 Uiso 1 1 calc R
C24 C 0.1297(2) 0.4345(2) 0.5567(2) 0.0421(6) Uani 1 1 d .
H24 H 0.0637 0.4778 0.5896 0.051 Uiso 1 1 calc R
C25 C 0.2004(2) 0.4719(2) 0.4520(2) 0.0384(5) Uani 1 1 d .
H25 H 0.1822 0.5405 0.4128 0.046 Uiso 1 1 calc R
C26 C 0.2983(2) 0.41028(17) 0.40291(17) 0.0288(4) Uani 1 1 d .
H26 H 0.3473 0.4366 0.3306 0.035 Uiso 1 1 calc R
C31 C 0.1938(2) 0.10199(18) 0.21821(16) 0.0264(4) Uani 1 1 d .
C32 C 0.1181(2) 0.0045(2) 0.2630(2) 0.0403(5) Uani 1 1 d .
H32 H 0.1479 -0.0547 0.3069 0.048 Uiso 1 1 calc R
C33 C -0.0009(3) -0.0061(3) 0.2433(2) 0.0511(7) Uani 1 1 d .
H33 H -0.0517 -0.0732 0.2727 0.061 Uiso 1 1 calc R
C34 C -0.0461(2) 0.0798(3) 0.1815(2) 0.0473(7) Uani 1 1 d .
H34 H -0.1279 0.0720 0.1686 0.057 Uiso 1 1 calc R
C35 C 0.0271(2) 0.1771(2) 0.13842(19) 0.0421(6) Uani 1 1 d .
H35 H -0.0048 0.2363 0.0961 0.051 Uiso 1 1 calc R
C36 C 0.1478(2) 0.18938(19) 0.15629(17) 0.0316(5) Uani 1 1 d .
H36 H 0.1981 0.2567 0.1265 0.038 Uiso 1 1 calc R
C41 C 0.4783(2) 0.05075(17) 0.15624(15) 0.0266(4) Uani 1 1 d .
C42 C 0.4585(3) -0.0585(2) 0.1656(2) 0.0403(5) Uani 1 1 d .
H42 H 0.3753 -0.0956 0.2091 0.048 Uiso 1 1 calc R
C43 C 0.5600(3) -0.1134(2) 0.1116(2) 0.0517(7) Uani 1 1 d .
H43 H 0.5468 -0.1883 0.1184 0.062 Uiso 1 1 calc R
C44 C 0.6801(3) -0.0591(2) 0.0480(2) 0.0486(7) Uani 1 1 d .
H44 H 0.7502 -0.0971 0.0118 0.058 Uiso 1 1 calc R
C45 C 0.6997(3) 0.0497(2) 0.03635(19) 0.0442(6) Uani 1 1 d .
H45 H 0.7824 0.0866 -0.0086 0.053 Uiso 1 1 calc R
C46 C 0.5986(2) 0.1053(2) 0.09030(17) 0.0341(5) Uani 1 1 d .
H46 H 0.6117 0.1805 0.0821 0.041 Uiso 1 1 calc R
Cl3 Cl 0.11350(6) 0.45328(5) 0.21668(5) 0.04119(13) Uani 1 1 d .
Cl4 Cl 0.21037(7) 0.64235(5) -0.02645(5) 0.04374(14) Uani 1 1 d .
Cl5 Cl 0.18195(7) 0.72189(5) 0.20148(5) 0.04553(15) Uani 1 1 d .
Cl6 Cl 0.44317(6) 0.56788(6) 0.10663(5) 0.05110(17) Uani 1 1 d .
Al Al 0.23709(7) 0.59620(5) 0.12440(5) 0.02976(14) Uani 1 1 d .
Cl1S Cl 0.62023(9) 0.52944(7) 0.31385(7) 0.0702(2) Uani 1 1 d .
Cl2S Cl 0.81053(12) 0.66896(10) 0.12822(8) 0.0996(4) Uani 1 1 d .
C1S C 0.7619(4) 0.5335(3) 0.2102(4) 0.0823(12) Uani 1 1 d .
H1SA H 0.7460 0.4877 0.1682 0.099 Uiso 1 1 calc R
H1SB H 0.8361 0.5032 0.2367 0.099 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'
Al Al 0.0645 0.0514 '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
Cl2 Sb P1 87.147(17) .
Cl2 Sb P2 82.286(18) .
P1 Sb P2 80.933(16) .
Cl2 Sb Cl1 162.004(19) .
P1 Sb Cl1 78.995(15) .
P2 Sb Cl1 84.222(15) .
Cl2 Sb Cl1 104.095(16) 2_656
P1 Sb Cl1 80.755(14) 2_656
P2 Sb Cl1 160.254(15) 2_656
Cl1 Sb Cl1 85.096(14) 2_656
C21 P1 C11 108.04(9) .
C21 P1 C1 110.00(9) .
C11 P1 C1 106.77(9) .
C21 P1 Sb 109.54(7) .
C11 P1 Sb 118.64(6) .
C1 P1 Sb 103.59(7) .
C41 P2 C31 109.41(9) .
C41 P2 C2 110.89(10) .
C31 P2 C2 108.24(10) .
C41 P2 Sb 110.70(7) .
C31 P2 Sb 112.92(7) .
C2 P2 Sb 104.59(7) .
C2 C1 P1 113.72(14) .
C1 C2 P2 112.40(14) .
C16 C11 C12 119.46(18) .
C16 C11 P1 119.27(15) .
C12 C11 P1 121.25(15) .
C13 C12 C11 119.9(2) .
C14 C13 C12 120.3(2) .
C13 C14 C15 120.1(2) .
C14 C15 C16 120.3(2) .
C15 C16 C11 119.9(2) .
C26 C21 C22 119.94(18) .
C26 C21 P1 121.18(16) .
C22 C21 P1 118.87(15) .
C23 C22 C21 119.9(2) .
C22 C23 C24 119.8(2) .
C25 C24 C23 120.4(2) .
C24 C25 C26 120.6(2) .
C25 C26 C21 119.3(2) .
C32 C31 C36 119.9(2) .
C32 C31 P2 119.89(17) .
C36 C31 P2 120.25(17) .
C33 C32 C31 119.8(2) .
C34 C33 C32 120.5(3) .
C35 C34 C33 120.1(2) .
C34 C35 C36 120.5(2) .
C31 C36 C35 119.3(2) .
C46 C41 C42 119.8(2) .
C46 C41 P2 121.63(17) .
C42 C41 P2 118.37(17) .
C43 C42 C41 120.0(2) .
C44 C43 C42 119.8(3) .
C45 C44 C43 120.7(2) .
C44 C45 C46 120.0(2) .
C41 C46 C45 119.8(2) .
Cl6 Al Cl5 107.60(4) .
Cl6 Al Cl3 111.04(4) .
Cl5 Al Cl3 109.24(4) .
Cl6 Al Cl4 109.38(4) .
Cl5 Al Cl4 111.19(4) .
Cl3 Al Cl4 108.39(4) .
Cl1S C1S Cl2S 112.08(19) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb Cl2 2.4640(5) .
Sb P1 2.6121(5) .
Sb P2 2.6164(5) .
Sb Cl1 2.6791(5) .
Sb Cl1 3.1255(5) 2_656
P1 C21 1.7956(19) .
P1 C11 1.811(2) .
P1 C1 1.822(2) .
P2 C41 1.799(2) .
P2 C31 1.801(2) .
P2 C2 1.824(2) .
C1 C2 1.535(3) .
C11 C16 1.395(3) .
C11 C12 1.400(3) .
C12 C13 1.390(3) .
C13 C14 1.382(3) .
C14 C15 1.384(3) .
C15 C16 1.390(3) .
C21 C26 1.394(3) .
C21 C22 1.397(3) .
C22 C23 1.384(3) .
C23 C24 1.387(4) .
C24 C25 1.375(4) .
C25 C26 1.390(3) .
C31 C32 1.390(3) .
C31 C36 1.392(3) .
C32 C33 1.386(3) .
C33 C34 1.374(4) .
C34 C35 1.374(4) .
C35 C36 1.394(3) .
C41 C46 1.387(3) .
C41 C42 1.389(3) .
C42 C43 1.384(4) .
C43 C44 1.378(4) .
C44 C45 1.375(4) .
C45 C46 1.388(3) .
Cl3 Al 2.1368(9) .
Cl4 Al 2.1403(9) .
Cl5 Al 2.1350(9) .
Cl6 Al 2.1300(9) .
Cl1S C1S 1.708(4) .
Cl2S C1S 1.793(4) .
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
Cl2 Sb P1 C21 21.29(7) .
P2 Sb P1 C21 103.93(7) .
Cl1 Sb P1 C21 -170.25(7) .
Cl1 Sb P1 C21 -83.49(7) 2_656
Cl2 Sb P1 C11 145.92(8) .
P2 Sb P1 C11 -131.45(8) .
Cl1 Sb P1 C11 -45.62(7) .
Cl1 Sb P1 C11 41.13(7) 2_656
Cl2 Sb P1 C1 -96.04(7) .
P2 Sb P1 C1 -13.40(7) .
Cl1 Sb P1 C1 72.43(7) .
Cl1 Sb P1 C1 159.18(7) 2_656
Cl2 Sb P2 C41 -163.21(8) .
P1 Sb P2 C41 108.47(8) .
Cl1 Sb P2 C41 28.73(8) .
Cl1 Sb P2 C41 86.30(9) 2_656
Cl2 Sb P2 C31 -40.15(8) .
P1 Sb P2 C31 -128.48(8) .
Cl1 Sb P2 C31 151.78(8) .
Cl1 Sb P2 C31 -150.64(8) 2_656
Cl2 Sb P2 C2 77.31(7) .
P1 Sb P2 C2 -11.01(7) .
Cl1 Sb P2 C2 -90.75(7) .
Cl1 Sb P2 C2 -33.18(9) 2_656
C21 P1 C1 C2 -73.45(16) .
C11 P1 C1 C2 169.56(14) .
Sb P1 C1 C2 43.55(15) .
P1 C1 C2 P2 -59.08(17) .
C41 P2 C2 C1 -78.71(16) .
C31 P2 C2 C1 161.28(14) .
Sb P2 C2 C1 40.64(15) .
C21 P1 C11 C16 29.85(19) .
C1 P1 C11 C16 148.13(16) .
Sb P1 C11 C16 -95.50(16) .
C21 P1 C11 C12 -148.26(16) .
C1 P1 C11 C12 -29.99(19) .
Sb P1 C11 C12 86.39(17) .
C16 C11 C12 C13 0.1(3) .
P1 C11 C12 C13 178.18(16) .
C11 C12 C13 C14 0.0(3) .
C12 C13 C14 C15 0.0(4) .
C13 C14 C15 C16 -0.2(4) .
C14 C15 C16 C11 0.3(3) .
C12 C11 C16 C15 -0.2(3) .
P1 C11 C16 C15 -178.40(17) .
C11 P1 C21 C26 104.23(17) .
C1 P1 C21 C26 -12.0(2) .
Sb P1 C21 C26 -125.20(16) .
C11 P1 C21 C22 -77.05(18) .
C1 P1 C21 C22 166.76(16) .
Sb P1 C21 C22 53.52(17) .
C26 C21 C22 C23 -1.2(3) .
P1 C21 C22 C23 -179.89(17) .
C21 C22 C23 C24 0.7(3) .
C22 C23 C24 C25 0.2(4) .
C23 C24 C25 C26 -0.8(4) .
C24 C25 C26 C21 0.4(3) .
C22 C21 C26 C25 0.6(3) .
P1 C21 C26 C25 179.30(17) .
C41 P2 C31 C32 78.2(2) .
C2 P2 C31 C32 -160.82(18) .
Sb P2 C31 C32 -45.5(2) .
C41 P2 C31 C36 -101.26(18) .
C2 P2 C31 C36 19.7(2) .
Sb P2 C31 C36 134.97(15) .
C36 C31 C32 C33 1.8(4) .
P2 C31 C32 C33 -177.7(2) .
C31 C32 C33 C34 -1.3(4) .
C32 C33 C34 C35 0.2(4) .
C33 C34 C35 C36 0.4(4) .
C32 C31 C36 C35 -1.2(3) .
P2 C31 C36 C35 178.29(17) .
C34 C35 C36 C31 0.1(3) .
C31 P2 C41 C46 127.07(18) .
C2 P2 C41 C46 7.8(2) .
Sb P2 C41 C46 -107.86(17) .
C31 P2 C41 C42 -58.5(2) .
C2 P2 C41 C42 -177.84(17) .
Sb P2 C41 C42 66.54(18) .
C46 C41 C42 C43 1.8(4) .
P2 C41 C42 C43 -172.7(2) .
C41 C42 C43 C44 -0.5(4) .
C42 C43 C44 C45 -1.0(4) .
C43 C44 C45 C46 1.0(4) .
C42 C41 C46 C45 -1.8(3) .
P2 C41 C46 C45 172.57(18) .
C44 C45 C46 C41 0.3(4) .
