#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:33:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179485 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/82/4338239.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_4338239
loop_
_publ_author_name
'Chitnis, Saurabh S.'
'Burford, Neil'
'McDonald, Robert'
'Ferguson, Michael J.'
_publ_section_title
;
 Prototypical Phosphine Complexes of Antimony(III).
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5359
_journal_page_last               5372
_journal_paper_doi               10.1021/ic500723y
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C36 H66 Cl3 P2 Sb'
_chemical_formula_sum            'C36 H66 Cl3 P2 Sb'
_chemical_formula_weight         788.93
_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                115.1065(7)
_cell_angle_beta                 104.6530(7)
_cell_angle_gamma                94.0515(8)
_cell_formula_units_Z            1
_cell_length_a                   9.7577(7)
_cell_length_b                   10.3383(7)
_cell_length_c                   11.2342(8)
_cell_measurement_reflns_used    5813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.20
_cell_volume                     972.13(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0140
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8741
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.8504
_exptl_absorpt_correction_T_min  0.7056
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0250
_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)+(0.0384P)²+0.1634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                4049
_reflns_number_total             4453
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic500723y_si_008.cif
_cod_data_source_block           vic1341
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4338238--4338252.cif.
;
_cod_database_code               4338239
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb 0.0025(2) -0.01792(13) -0.00884(18) 0.02225(18) Uani 0.50 1 d P . -1
Cl1 Cl 0.18015(6) 0.08243(6) -0.09658(5) 0.04300(12) Uani 1 1 d . . .
Cl2 Cl -0.00793(9) 0.23084(9) 0.11754(8) 0.02958(17) Uani 0.50 1 d P A -1
P P 0.23187(4) 0.02701(4) 0.22840(4) 0.02158(9) Uani 1 1 d . . .
C11 C 0.28309(18) -0.14857(17) 0.20923(17) 0.0259(3) Uani 1 1 d . . .
H11 H 0.3695 -0.1262 0.2904 0.031 Uiso 1 1 calc R . .
C12 C 0.1623(2) -0.24990(19) 0.21152(19) 0.0314(4) Uani 1 1 d . . .
H12A H 0.1424 -0.2018 0.3008 0.038 Uiso 1 1 calc R . .
H12B H 0.0728 -0.2676 0.1366 0.038 Uiso 1 1 calc R . .
C13 C 0.2035(2) -0.3957(2) 0.1926(2) 0.0399(4) Uani 1 1 d . . .
H13A H 0.2870 -0.3791 0.2727 0.048 Uiso 1 1 calc R . .
H13B H 0.1214 -0.4602 0.1898 0.048 Uiso 1 1 calc R . .
C14 C 0.2423(3) -0.4702(2) 0.0604(2) 0.0482(5) Uani 1 1 d . . .
H14A H 0.1567 -0.4938 -0.0204 0.058 Uiso 1 1 calc R . .
H14B H 0.2716 -0.5626 0.0523 0.058 Uiso 1 1 calc R . .
C15 C 0.3653(3) -0.3714(2) 0.0608(3) 0.0649(8) Uani 1 1 d . . .
H15A H 0.3877 -0.4203 -0.0271 0.078 Uiso 1 1 calc R . .
H15B H 0.4528 -0.3541 0.1376 0.078 Uiso 1 1 calc R . .
C16 C 0.3269(3) -0.2246(2) 0.0777(2) 0.0541(6) Uani 1 1 d . . .
H16A H 0.2460 -0.2407 -0.0042 0.065 Uiso 1 1 calc R . .
H16B H 0.4113 -0.1609 0.0829 0.065 Uiso 1 1 calc R . .
C21 C 0.18562(17) 0.09802(17) 0.39162(16) 0.0243(3) Uani 1 1 d . . .
H21 H 0.1086 0.0190 0.3774 0.029 Uiso 1 1 calc R . .
C22 C 0.1163(2) 0.2320(2) 0.4223(2) 0.0357(4) Uani 1 1 d . . .
H22A H 0.1883 0.3168 0.4421 0.043 Uiso 1 1 calc R . .
H22B H 0.0345 0.2135 0.3403 0.043 Uiso 1 1 calc R . .
C23 C 0.0620(2) 0.2662(2) 0.5466(2) 0.0436(5) Uani 1 1 d . . .
H23A H 0.0234 0.3567 0.5686 0.052 Uiso 1 1 calc R . .
H23B H -0.0182 0.1860 0.5219 0.052 Uiso 1 1 calc R . .
C24 C 0.1799(2) 0.2851(2) 0.6736(2) 0.0416(5) Uani 1 1 d . . .
H24A H 0.2543 0.3731 0.7060 0.050 Uiso 1 1 calc R . .
H24B H 0.1379 0.2996 0.7488 0.050 Uiso 1 1 calc R . .
C25 C 0.2497(2) 0.1533(2) 0.64223(18) 0.0382(4) Uani 1 1 d . . .
H25A H 0.1778 0.0675 0.6205 0.046 Uiso 1 1 calc R . .
H25B H 0.3303 0.1712 0.7250 0.046 Uiso 1 1 calc R . .
C26 C 0.30743(18) 0.12062(19) 0.52018(16) 0.0284(3) Uani 1 1 d . . .
H26A H 0.3488 0.0317 0.4995 0.034 Uiso 1 1 calc R . .
H26B H 0.3854 0.2028 0.5447 0.034 Uiso 1 1 calc R . .
C31 C 0.39747(17) 0.13997(18) 0.24348(17) 0.0265(3) Uani 1 1 d . . .
H31 H 0.4020 0.1024 0.1469 0.032 Uiso 1 1 calc R . .
C32 C 0.3881(2) 0.2998(2) 0.2894(3) 0.0439(5) Uani 1 1 d . . .
H32A H 0.3904 0.3464 0.3873 0.053 Uiso 1 1 calc R . .
H32B H 0.2955 0.3063 0.2326 0.053 Uiso 1 1 calc R . .
C33 C 0.5148(2) 0.3805(3) 0.2733(4) 0.0643(8) Uani 1 1 d . . .
H33A H 0.5070 0.3395 0.1740 0.077 Uiso 1 1 calc R . .
H33B H 0.5096 0.4848 0.3073 0.077 Uiso 1 1 calc R . .
C34 C 0.6592(2) 0.3671(2) 0.3532(3) 0.0527(6) Uani 1 1 d . . .
H34A H 0.7385 0.4149 0.3362 0.063 Uiso 1 1 calc R . .
H34B H 0.6719 0.4176 0.4536 0.063 Uiso 1 1 calc R . .
C35 C 0.66738(19) 0.2094(2) 0.3101(2) 0.0410(4) Uani 1 1 d . . .
H35A H 0.7603 0.2034 0.3667 0.049 Uiso 1 1 calc R . .
H35B H 0.6645 0.1614 0.2119 0.049 Uiso 1 1 calc R . .
C36 C 0.54248(17) 0.1291(2) 0.3276(2) 0.0323(4) Uani 1 1 d . . .
H36A H 0.5491 0.1723 0.4266 0.039 Uiso 1 1 calc R . .
H36B H 0.5490 0.0253 0.2960 0.039 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_1
_geom_angle_site_symmetry_3
Cl2 Sb Cl1 84.45(6) . .
Cl2 Sb Cl1 87.68(6) . 2
Cl1 Sb Cl1 172.12(4) . 2
Cl2 Sb P 86.41(5) . .
Cl1 Sb P 90.60(6) . .
Cl1 Sb P 89.42(6) 2 .
Cl2 Sb P 86.56(5) . 2
Cl1 Sb P 89.17(6) . 2
Cl1 Sb P 89.85(6) 2 2
P Sb P 172.95(4) . 2
C21 P C31 112.27(8) . .
C21 P C11 103.71(7) . .
C31 P C11 104.82(7) . .
C21 P Sb 114.55(6) . .
C31 P Sb 110.34(7) . .
C11 P Sb 110.52(6) . .
C12 C11 C16 110.98(14) . .
C12 C11 P 111.64(11) . .
C16 C11 P 111.39(13) . .
C13 C12 C11 111.53(15) . .
C14 C13 C12 111.30(17) . .
C13 C14 C15 110.22(17) . .
C14 C15 C16 111.6(2) . .
C15 C16 C11 111.00(19) . .
C22 C21 C26 110.61(14) . .
C22 C21 P 115.09(12) . .
C26 C21 P 115.21(11) . .
C23 C22 C21 110.28(16) . .
C24 C23 C22 112.47(15) . .
C25 C24 C23 111.09(16) . .
C24 C25 C26 111.32(16) . .
C25 C26 C21 110.48(14) . .
C32 C31 C36 109.88(14) . .
C32 C31 P 113.07(12) . .
C36 C31 P 117.41(11) . .
C31 C32 C33 110.31(17) . .
C34 C33 C32 111.39(19) . .
C35 C34 C33 110.83(18) . .
C34 C35 C36 111.34(16) . .
C35 C36 C31 110.29(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb Cl2 2.3773(12) .
Sb Cl1 2.556(2) .
Sb Cl1 2.568(2) 2
Sb P 2.848(2) .
Sb P 2.871(2) 2
P C21 1.8514(16) .
P C31 1.8522(16) .
P C11 1.8553(17) .
C11 C12 1.533(2) .
C11 C16 1.538(2) .
C12 C13 1.529(2) .
C13 C14 1.516(3) .
C14 C15 1.518(3) .
C15 C16 1.533(3) .
C21 C22 1.530(2) .
C21 C26 1.536(2) .
C22 C23 1.529(3) .
C23 C24 1.516(3) .
C24 C25 1.514(3) .
C25 C26 1.528(2) .
C31 C32 1.526(2) .
C31 C36 1.531(2) .
C32 C33 1.533(3) .
C33 C34 1.519(3) .
C34 C35 1.506(3) .
C35 C36 1.526(3) .
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 P C21 55.27(9) .
Cl1 Sb P C21 139.68(6) .
Cl1 Sb P C21 -32.44(7) 2
P Sb P C21 51.6(7) 2
Cl2 Sb P C31 -72.58(8) .
Cl1 Sb P C31 11.83(7) .
Cl1 Sb P C31 -160.29(6) 2
P Sb P C31 -76.2(7) 2
Cl2 Sb P C11 171.96(7) .
Cl1 Sb P C11 -103.63(6) .
Cl1 Sb P C11 84.25(6) 2
P Sb P C11 168.3(7) 2
C21 P C11 C12 55.75(13) .
C31 P C11 C12 173.66(12) .
Sb P C11 C12 -67.47(13) .
C21 P C11 C16 -179.56(14) .
C31 P C11 C16 -61.66(15) .
Sb P C11 C16 57.21(15) .
C16 C11 C12 C13 53.9(2) .
P C11 C12 C13 178.80(13) .
C11 C12 C13 C14 -56.2(2) .
C12 C13 C14 C15 57.4(3) .
C13 C14 C15 C16 -57.5(3) .
C14 C15 C16 C11 55.8(3) .
C12 C11 C16 C15 -53.5(3) .
P C11 C16 C15 -178.56(17) .
C31 P C21 C22 76.50(14) .
C11 P C21 C22 -170.90(12) .
Sb P C21 C22 -50.36(14) .
C31 P C21 C26 -54.04(14) .
C11 P C21 C26 58.56(13) .
Sb P C21 C26 179.10(11) .
C26 C21 C22 C23 -55.98(19) .
P C21 C22 C23 171.29(12) .
C21 C22 C23 C24 55.2(2) .
C22 C23 C24 C25 -54.8(2) .
C23 C24 C25 C26 55.3(2) .
C24 C25 C26 C21 -56.9(2) .
C22 C21 C26 C25 57.27(19) .
P C21 C26 C25 -170.06(12) .
C21 P C31 C32 -56.39(15) .
C11 P C31 C32 -168.30(14) .
Sb P C31 C32 72.70(14) .
C21 P C31 C36 73.19(15) .
C11 P C31 C36 -38.72(15) .
Sb P C31 C36 -157.71(12) .
C36 C31 C32 C33 57.4(2) .
P C31 C32 C33 -169.28(17) .
C31 C32 C33 C34 -56.5(3) .
C32 C33 C34 C35 55.7(3) .
C33 C34 C35 C36 -56.2(3) .
C34 C35 C36 C31 57.7(2) .
C32 C31 C36 C35 -58.0(2) .
P C31 C36 C35 170.94(13) .
