#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317920.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_4317920
loop_
_publ_author_name
'Praveen Kommana'
'Sudha Kumaraswamy'
'J. J. Vittal'
'K. C. Kumara Swamy'
_publ_section_title
;
 Apical versus Equatorial Disposition of Substituents in
 Tetraoxyphosphoranes Bearing a 1,3,2-Dioxaphosphocin Ring: Implications
 on Apicophilicity in Trigonal Bipyramidal Phosphorus
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2356
_journal_page_last               2363
_journal_paper_doi               10.1021/ic010935w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C33.5 H38 Cl4 N O4 P S'
_chemical_formula_weight         723.48
_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                72.986(18)
_cell_angle_beta                 78.85(4)
_cell_angle_gamma                73.25(3)
_cell_formula_units_Z            2
_cell_length_a                   9.563(2)
_cell_length_b                   12.993(2)
_cell_length_c                   15.994(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1806.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6348
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        5%
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0961P)²+4.9768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2582
_reflns_number_gt                3248
_reflns_number_total             6348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010935w_5.cif
_cod_data_source_block           compd5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+4.9768P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+4.9768P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1806.7(6)
_cod_original_formula_sum        'C33.50 H38 Cl4 N O4 P S'
_cod_database_code               4317920
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.1840(2) 0.78563(14) 0.71821(9) 0.0633(5) Uani 1 d . . .
S S 0.1617(7) 0.5866(4) 0.9920(2) 0.277(3) Uani 1 d . . .
Cl1 Cl 0.4761(3) 0.99390(18) 0.76329(13) 0.0981(7) Uani 1 d . . .
Cl2 Cl 0.4928(3) 1.19817(18) 0.59510(15) 0.1074(8) Uani 1 d . . .
Cl3 Cl 0.3514(2) 1.21699(16) 0.42995(12) 0.0932(7) Uani 1 d . . .
Cl4 Cl 0.1798(2) 1.04147(16) 0.43341(10) 0.0850(6) Uani 1 d . . .
O1 O 0.0157(5) 0.8494(4) 0.7303(2) 0.0665(12) Uani 1 d . . .
O2 O 0.2304(5) 0.6777(3) 0.6815(2) 0.0620(11) Uani 1 d . . .
O3 O 0.2999(5) 0.8463(3) 0.7366(2) 0.0658(12) Uani 1 d . . .
O4 O 0.1926(5) 0.8608(3) 0.6106(2) 0.0668(12) Uani 1 d . . .
N N 0.1914(6) 0.7088(4) 0.8268(3) 0.0685(15) Uani 1 d . . .
C1 C -0.0984(7) 0.8178(5) 0.7956(4) 0.0609(16) Uani 1 d . . .
C2 C -0.1693(8) 0.8832(5) 0.8541(4) 0.0661(17) Uani 1 d . . .
C3 C -0.2823(9) 0.8471(7) 0.9140(4) 0.082(2) Uani 1 d . . .
H3 H -0.3330 0.8882 0.9542 0.098 Uiso 1 calc R . .
C4 C -0.3222(9) 0.7506(6) 0.9156(4) 0.081(2) Uani 1 d . . .
C5 C -0.2521(8) 0.6925(6) 0.8532(4) 0.075(2) Uani 1 d . . .
H5 H -0.2818 0.6307 0.8523 0.090 Uiso 1 calc R . .
C6 C -0.1379(7) 0.7243(5) 0.7916(4) 0.0612(16) Uani 1 d . . .
C7 C -0.0664(7) 0.6613(5) 0.7220(4) 0.0653(18) Uani 1 d . . .
H7A H -0.0329 0.7127 0.6698 0.078 Uiso 1 calc R . .
H7B H -0.1408 0.6351 0.7065 0.078 Uiso 1 calc R . .
C8 C 0.0637(8) 0.5618(5) 0.7476(4) 0.0616(17) Uani 1 d . . .
C9 C 0.0423(9) 0.4560(6) 0.7895(4) 0.0720(19) Uani 1 d . . .
H9 H -0.0534 0.4476 0.8045 0.086 Uiso 1 calc R . .
C10 C 0.1588(10) 0.3618(6) 0.8097(5) 0.081(2) Uani 1 d . . .
C11 C 0.3047(9) 0.3718(6) 0.7849(4) 0.0742(19) Uani 1 d . . .
H11 H 0.3820 0.3088 0.7960 0.089 Uiso 1 calc R . .
C12 C 0.3353(8) 0.4763(6) 0.7432(4) 0.0654(17) Uani 1 d . . .
C13 C 0.2114(8) 0.5676(5) 0.7276(3) 0.0602(17) Uani 1 d . . .
C14 C -0.1330(9) 0.9924(6) 0.8546(5) 0.077(2) Uani 1 d . . .
C15 C 0.0191(10) 0.9629(6) 0.8858(5) 0.090(2) Uani 1 d . . .
H15A H 0.0219 0.9068 0.9405 0.135 Uiso 1 calc R . .
H15B H 0.0371 1.0280 0.8942 0.135 Uiso 1 calc R . .
H15C H 0.0932 0.9355 0.8424 0.135 Uiso 1 calc R . .
C16 C -0.1363(12) 1.0739(6) 0.7620(5) 0.105(3) Uani 1 d . . .
H16A H -0.0604 1.0418 0.7215 0.158 Uiso 1 calc R . .
H16B H -0.1202 1.1424 0.7647 0.158 Uiso 1 calc R . .
H16C H -0.2303 1.0881 0.7423 0.158 Uiso 1 calc R . .
C17 C -0.2470(11) 1.0566(8) 0.9165(6) 0.116(3) Uani 1 d . . .
H17A H -0.3425 1.0765 0.8972 0.173 Uiso 1 calc R . .
H17B H -0.2195 1.1226 0.9150 0.173 Uiso 1 calc R . .
H17C H -0.2496 1.0103 0.9755 0.173 Uiso 1 calc R . .
C18 C -0.4486(12) 0.7172(9) 0.9818(6) 0.129(4) Uani 1 d . . .
H18A H -0.5305 0.7267 0.9513 0.193 Uiso 1 calc R . .
H18B H -0.4775 0.7630 1.0226 0.193 Uiso 1 calc R . .
H18C H -0.4178 0.6408 1.0131 0.193 Uiso 1 calc R . .
C19 C 0.1323(11) 0.2464(7) 0.8543(6) 0.117(3) Uani 1 d . . .
H19A H 0.0592 0.2506 0.9044 0.176 Uiso 1 calc R . .
H19B H 0.2224 0.1960 0.8731 0.176 Uiso 1 calc R . .
H19C H 0.0987 0.2204 0.8133 0.176 Uiso 1 calc R . .
C20 C 0.4968(8) 0.4820(6) 0.7118(4) 0.0721(19) Uani 1 d . . .
C21 C 0.5368(9) 0.5620(6) 0.7539(5) 0.086(2) Uani 1 d . . .
H21A H 0.4813 0.6365 0.7316 0.130 Uiso 1 calc R . .
H21B H 0.6400 0.5585 0.7395 0.130 Uiso 1 calc R . .
H21C H 0.5136 0.5403 0.8167 0.130 Uiso 1 calc R . .
C22 C 0.5146(10) 0.5266(7) 0.6106(5) 0.095(3) Uani 1 d . . .
H22A H 0.4928 0.4764 0.5841 0.143 Uiso 1 calc R . .
H22B H 0.6139 0.5326 0.5904 0.143 Uiso 1 calc R . .
H22C H 0.4482 0.5984 0.5945 0.143 Uiso 1 calc R . .
C23 C 0.6098(10) 0.3659(7) 0.7366(6) 0.101(3) Uani 1 d . . .
H23A H 0.6063 0.3400 0.7994 0.151 Uiso 1 calc R . .
H23B H 0.7071 0.3732 0.7114 0.151 Uiso 1 calc R . .
H23C H 0.5847 0.3136 0.7139 0.151 Uiso 1 calc R . .
C24 C 0.3225(7) 0.9359(5) 0.6691(4) 0.0624(16) Uani 1 d . . .
C25 C 0.3952(8) 1.0136(5) 0.6708(4) 0.0674(17) Uani 1 d . . .
C26 C 0.4052(8) 1.0987(5) 0.5958(4) 0.0734(19) Uani 1 d . . .
C27 C 0.3381(8) 1.1099(5) 0.5227(4) 0.0697(18) Uani 1 d . . .
C28 C 0.2657(7) 1.0303(5) 0.5219(4) 0.0637(17) Uani 1 d . . .
C29 C 0.2555(7) 0.9468(5) 0.5963(4) 0.0587(15) Uani 1 d . . .
C30 C 0.1802(10) 0.6573(7) 0.8960(5) 0.090(2) Uani 1 d . . .
C31 C 0.924(6) 0.427(9) 0.501(5) 0.56(5) Uani 1 d D . .
C32 C 0.922(3) 0.530(9) 0.438(3) 0.76(6) Uani 1 d D . .
C33 C 1.034(10) 0.378(5) 0.557(2) 0.55(4) Uani 1 d D . .
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
O1 P O2 119.8(2) . . ?
O1 P O3 115.1(2) . . ?
O2 P O3 124.8(3) . . ?
O1 P O4 88.1(2) . . ?
O2 P O4 86.8(2) . . ?
O3 P O4 89.87(19) . . ?
O1 P N 96.2(3) . . ?
O2 P N 93.0(2) . . ?
O3 P N 86.1(2) . . ?
O4 P N 175.0(3) . . ?
C1 O1 P 128.8(4) . . ?
C13 O2 P 127.6(3) . . ?
C24 O3 P 113.2(3) . . ?
C29 O4 P 112.7(3) . . ?
C30 N P 171.5(6) . . ?
C6 C1 C2 124.4(6) . . ?
C6 C1 O1 115.3(5) . . ?
C2 C1 O1 120.1(5) . . ?
C3 C2 C1 115.9(6) . . ?
C3 C2 C14 119.4(6) . . ?
C1 C2 C14 124.7(6) . . ?
C2 C3 C4 122.1(7) . . ?
C5 C4 C3 119.1(6) . . ?
C5 C4 C18 121.5(7) . . ?
C3 C4 C18 119.3(7) . . ?
C4 C5 C6 121.5(6) . . ?
C5 C6 C1 116.9(6) . . ?
C5 C6 C7 120.3(5) . . ?
C1 C6 C7 122.7(5) . . ?
C6 C7 C8 115.9(5) . . ?
C9 C8 C13 115.1(7) . . ?
C9 C8 C7 121.1(6) . . ?
C13 C8 C7 123.7(5) . . ?
C8 C9 C10 122.9(6) . . ?
C9 C10 C11 119.6(6) . . ?
C9 C10 C19 121.8(7) . . ?
C11 C10 C19 118.6(8) . . ?
C10 C11 C12 120.9(7) . . ?
C11 C12 C13 115.9(6) . . ?
C11 C12 C20 118.9(7) . . ?
C13 C12 C20 125.0(5) . . ?
C8 C13 C12 125.6(5) . . ?
C8 C13 O2 113.8(6) . . ?
C12 C13 O2 120.4(5) . . ?
C15 C14 C16 110.8(7) . . ?
C15 C14 C17 108.5(6) . . ?
C16 C14 C17 105.4(7) . . ?
C15 C14 C2 108.6(6) . . ?
C16 C14 C2 111.0(5) . . ?
C17 C14 C2 112.6(6) . . ?
C12 C20 C22 108.5(6) . . ?
C12 C20 C21 110.1(6) . . ?
C22 C20 C21 109.1(6) . . ?
C12 C20 C23 113.1(6) . . ?
C22 C20 C23 108.4(7) . . ?
C21 C20 C23 107.6(6) . . ?
O3 C24 C29 112.3(4) . . ?
O3 C24 C25 126.6(5) . . ?
C29 C24 C25 121.0(5) . . ?
C26 C25 C24 117.8(6) . . ?
C26 C25 Cl1 123.9(5) . . ?
C24 C25 Cl1 118.3(5) . . ?
C25 C26 C27 121.3(5) . . ?
C25 C26 Cl2 119.5(5) . . ?
C27 C26 Cl2 119.1(5) . . ?
C26 C27 C28 120.1(5) . . ?
C26 C27 Cl3 120.5(4) . . ?
C28 C27 Cl3 119.2(5) . . ?
C29 C28 C27 118.2(6) . . ?
C29 C28 Cl4 119.9(4) . . ?
C27 C28 Cl4 121.8(5) . . ?
O4 C29 C28 128.7(5) . . ?
O4 C29 C24 109.8(5) . . ?
C28 C29 C24 121.4(5) . . ?
N C30 S 179.0(9) . . ?
C33 C31 C32 122(5) . . ?
C31 C32 C33 129(3) . 2_766 ?
C31 C33 C32 102(4) . 2_766 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P O1 1.588(5) . ?
P O2 1.591(4) . ?
P O3 1.644(4) . ?
P O4 1.713(4) . ?
P N 1.735(5) . ?
S C30 1.548(7) . ?
Cl1 C25 1.721(6) . ?
Cl2 C26 1.727(6) . ?
Cl3 C27 1.724(6) . ?
Cl4 C28 1.721(6) . ?
O1 C1 1.419(7) . ?
O2 C13 1.450(6) . ?
O3 C24 1.374(6) . ?
O4 C29 1.360(6) . ?
N C30 1.116(8) . ?
C1 C6 1.393(8) . ?
C1 C2 1.395(9) . ?
C2 C3 1.390(9) . ?
C2 C14 1.557(9) . ?
C3 C4 1.404(10) . ?
C4 C5 1.381(10) . ?
C4 C18 1.519(10) . ?
C5 C6 1.393(8) . ?
C6 C7 1.514(9) . ?
C7 C8 1.532(10) . ?
C8 C9 1.397(8) . ?
C8 C13 1.406(9) . ?
C9 C10 1.402(11) . ?
C10 C11 1.407(10) . ?
C10 C19 1.531(9) . ?
C11 C12 1.414(8) . ?
C12 C13 1.416(10) . ?
C12 C20 1.545(9) . ?
C14 C15 1.536(11) . ?
C14 C16 1.548(10) . ?
C14 C17 1.551(11) . ?
C20 C22 1.545(9) . ?
C20 C21 1.555(9) . ?
C20 C23 1.573(11) . ?
C24 C29 1.388(8) . ?
C24 C25 1.389(7) . ?
C25 C26 1.382(8) . ?
C26 C27 1.392(9) . ?
C27 C28 1.404(8) . ?
C28 C29 1.365(8) . ?
C31 C33 1.397(19) . ?
C31 C32 1.41(2) . ?
C32 C33 1.41(2) 2_766 ?
C33 C32 1.41(2) 2_766 ?
