#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/79/4317916.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_4317916
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            'C36 H38 Cl4 N O4 P'
_chemical_formula_weight         721.44
_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                105.74(4)
_cell_angle_beta                 101.57(2)
_cell_angle_gamma                104.65(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2190(14)
_cell_length_b                   11.192(6)
_cell_length_c                   17.157(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1749.3(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    0.0473
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6143
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0832P)²+2.4214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                3398
_reflns_number_total             6143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010935w_1.cif
_cod_data_source_block           compd1
_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^)+(0.0832P)^2^+2.4214P] 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^)+(0.0832P)^2^+2.4214P] 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        1749.3(10)
_cod_database_code               4317916
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 0.13801(14) 0.28773(12) 0.83508(8) 0.0409(3) Uani 1 d . . .
Cl1 Cl 0.46857(19) 0.68104(15) 0.85060(10) 0.0743(5) Uani 1 d . . .
Cl2 Cl 0.50785(17) 0.66398(15) 0.66949(11) 0.0673(5) Uani 1 d . . .
Cl3 Cl 0.33659(19) 0.40904(17) 0.51604(9) 0.0736(5) Uani 1 d . . .
Cl4 Cl 0.11483(17) 0.17563(15) 0.54128(8) 0.0637(4) Uani 1 d . . .
O1 O 0.1737(3) 0.1607(3) 0.84680(19) 0.0402(8) Uani 1 d . . .
O2 O -0.0249(4) 0.2752(3) 0.80724(19) 0.0449(8) Uani 1 d . . .
O3 O 0.2616(4) 0.4243(3) 0.8448(2) 0.0478(9) Uani 1 d . . .
O4 O 0.1347(4) 0.2309(3) 0.72767(19) 0.0435(8) Uani 1 d . . .
N N 0.1546(4) 0.3557(4) 0.9412(2) 0.0437(10) Uani 1 d . . .
C1 C 0.1604(5) 0.0430(4) 0.7837(3) 0.0396(11) Uani 1 d . . .
C2 C 0.2799(5) 0.0085(5) 0.7752(3) 0.0449(12) Uani 1 d . . .
C3 C 0.2574(6) -0.1087(5) 0.7121(4) 0.0545(14) Uani 1 d . . .
H3 H 0.3354 -0.1337 0.7047 0.065 Uiso 1 calc R . .
C4 C 0.1240(6) -0.1911(5) 0.6592(4) 0.0562(14) Uani 1 d . . .
C5 C 0.0087(6) -0.1548(5) 0.6748(3) 0.0539(14) Uani 1 d . . .
H5 H -0.0819 -0.2105 0.6429 0.065 Uiso 1 calc R . .
C6 C 0.0245(5) -0.0384(5) 0.7363(3) 0.0441(12) Uani 1 d . . .
C7 C -0.1053(5) -0.0046(5) 0.7500(3) 0.0502(13) Uani 1 d . . .
H7A H -0.0846 0.0476 0.8090 0.060 Uiso 1 calc R . .
H7B H -0.1811 -0.0853 0.7384 0.060 Uiso 1 calc R . .
C8 C -0.1564(5) 0.0707(5) 0.6950(3) 0.0452(12) Uani 1 d . . .
C9 C -0.2364(6) 0.0034(7) 0.6130(3) 0.0605(16) Uani 1 d . . .
H9 H -0.2622 -0.0876 0.5918 0.073 Uiso 1 calc R . .
C10 C -0.2797(6) 0.0720(7) 0.5604(4) 0.0647(17) Uani 1 d . . .
C11 C -0.2508(6) 0.2067(7) 0.5947(4) 0.0634(16) Uani 1 d . . .
H11 H -0.2845 0.2508 0.5607 0.076 Uiso 1 calc R . .
C12 C -0.1731(6) 0.2770(6) 0.6780(3) 0.0512(13) Uani 1 d . . .
C13 C -0.1197(5) 0.2067(5) 0.7252(3) 0.0465(12) Uani 1 d . . .
C14 C 0.4307(6) 0.0888(5) 0.8338(4) 0.0512(13) Uani 1 d . . .
C15 C 0.5420(7) 0.0322(7) 0.8081(5) 0.085(2) Uani 1 d . . .
H15A H 0.5488 0.0398 0.7545 0.128 Uiso 1 calc R . .
H15B H 0.5159 -0.0586 0.8034 0.128 Uiso 1 calc R . .
H15C H 0.6316 0.0797 0.8501 0.128 Uiso 1 calc R . .
C16 C 0.4752(7) 0.2295(6) 0.8317(5) 0.0739(19) Uani 1 d . . .
H16A H 0.4589 0.2268 0.7741 0.111 Uiso 1 calc R . .
H16B H 0.5738 0.2727 0.8614 0.111 Uiso 1 calc R . .
H16C H 0.4208 0.2770 0.8584 0.111 Uiso 1 calc R . .
C17 C 0.4363(7) 0.0951(9) 0.9236(4) 0.090(2) Uani 1 d . . .
H17A H 0.5303 0.1447 0.9600 0.135 Uiso 1 calc R . .
H17B H 0.4111 0.0078 0.9260 0.135 Uiso 1 calc R . .
H17C H 0.3712 0.1368 0.9419 0.135 Uiso 1 calc R . .
C18 C 0.1059(7) -0.3137(6) 0.5889(4) 0.0719(18) Uani 1 d . . .
H18A H 0.0099 -0.3708 0.5714 0.108 Uiso 1 calc R . .
H18B H 0.1682 -0.3576 0.6085 0.108 Uiso 1 calc R . .
H18C H 0.1282 -0.2910 0.5419 0.108 Uiso 1 calc R . .
C19 C -0.3561(8) 0.0005(8) 0.4657(4) 0.091(2) Uani 1 d . . .
H19A H -0.4204 0.0433 0.4470 0.137 Uiso 1 calc R . .
H19B H -0.4078 -0.0890 0.4566 0.137 Uiso 1 calc R . .
H19C H -0.2880 0.0026 0.4345 0.137 Uiso 1 calc R . .
C20 C -0.1542(7) 0.4268(6) 0.7145(4) 0.0580(15) Uani 1 d . . .
C21 C 0.0006(7) 0.5108(7) 0.7409(5) 0.080(2) Uani 1 d . . .
H21A H 0.0069 0.5987 0.7429 0.120 Uiso 1 calc R . .
H21B H 0.0454 0.4745 0.7006 0.120 Uiso 1 calc R . .
H21C H 0.0470 0.5122 0.7958 0.120 Uiso 1 calc R . .
C22 C -0.2343(9) 0.4710(9) 0.6476(5) 0.104(3) Uani 1 d . . .
H22A H -0.3331 0.4214 0.6302 0.155 Uiso 1 calc R . .
H22B H -0.1982 0.4563 0.5996 0.155 Uiso 1 calc R . .
H22C H -0.2216 0.5627 0.6713 0.155 Uiso 1 calc R . .
C23 C -0.2105(9) 0.4515(7) 0.7901(5) 0.088(2) Uani 1 d . . .
H23A H -0.3093 0.4021 0.7730 0.131 Uiso 1 calc R . .
H23B H -0.1977 0.5434 0.8132 0.131 Uiso 1 calc R . .
H23C H -0.1604 0.4249 0.8323 0.131 Uiso 1 calc R . .
C24 C 0.2937(5) 0.4339(5) 0.7723(3) 0.0418(11) Uani 1 d . . .
C25 C 0.3819(5) 0.5411(5) 0.7648(3) 0.0446(12) Uani 1 d . . .
C26 C 0.3951(5) 0.5336(5) 0.6836(3) 0.0479(13) Uani 1 d . . .
C27 C 0.3184(5) 0.4194(5) 0.6147(3) 0.0446(12) Uani 1 d . . .
C28 C 0.2241(5) 0.3119(5) 0.6243(3) 0.0429(12) Uani 1 d . . .
C29 C 0.2161(5) 0.3203(5) 0.7054(3) 0.0404(11) Uani 1 d . . .
C30 C 0.2920(8) 0.4334(8) 0.9998(4) 0.092(2) Uani 1 d . . .
H30A H 0.2873 0.4456 1.0566 0.138 Uiso 1 calc R . .
H30B H 0.3213 0.5173 0.9927 0.138 Uiso 1 calc R . .
H30C H 0.3589 0.3889 0.9891 0.138 Uiso 1 calc R . .
C31 C 0.0642(8) 0.2866(6) 0.9793(3) 0.0674(18) Uani 1 d . . .
C32 C 0.1058(13) 0.2090(8) 1.0211(5) 0.123(4) Uani 1 d . . .
H32 H 0.1909 0.1937 1.0203 0.147 Uiso 1 calc R . .
C33 C 0.023(2) 0.1527(11) 1.0646(9) 0.199(10) Uani 1 d . . .
H33 H 0.0517 0.0958 1.0896 0.238 Uiso 1 calc R . .
C34 C -0.089(2) 0.1754(13) 1.0718(7) 0.209(11) Uani 1 d . . .
H34 H -0.1395 0.1378 1.1035 0.251 Uiso 1 calc R . .
C35 C -0.1435(10) 0.2632(13) 1.0295(6) 0.153(5) Uani 1 d . . .
H35 H -0.2262 0.2809 1.0342 0.183 Uiso 1 calc R . .
C36 C -0.0611(8) 0.3162(11) 0.9826(5) 0.120(4) Uani 1 d . . .
H36 H -0.0889 0.3698 0.9544 0.144 Uiso 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'
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'
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'
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
O2 P O1 117.00(19) . . ?
O2 P O3 120.1(2) . . ?
O1 P O3 122.82(19) . . ?
O2 P N 92.93(19) . . ?
O1 P N 92.93(19) . . ?
O3 P N 87.71(19) . . ?
O2 P O4 90.28(17) . . ?
O1 P O4 89.45(17) . . ?
O3 P O4 86.96(16) . . ?
N P O4 174.63(19) . . ?
C1 O1 P 128.5(3) . . ?
C13 O2 P 125.8(3) . . ?
C24 O3 P 116.7(3) . . ?
C29 O4 P 113.2(3) . . ?
C31 N C30 112.1(5) . . ?
C31 N P 119.7(3) . . ?
C30 N P 119.8(4) . . ?
C6 C1 C2 122.7(5) . . ?
C6 C1 O1 117.1(4) . . ?
C2 C1 O1 120.1(4) . . ?
C3 C2 C1 116.4(5) . . ?
C3 C2 C14 119.5(5) . . ?
C1 C2 C14 124.0(5) . . ?
C2 C3 C4 123.5(5) . . ?
C5 C4 C3 117.0(5) . . ?
C5 C4 C18 121.6(5) . . ?
C3 C4 C18 121.4(6) . . ?
C6 C5 C4 122.1(5) . . ?
C5 C6 C1 118.1(5) . . ?
C5 C6 C7 119.4(5) . . ?
C1 C6 C7 122.4(4) . . ?
C6 C7 C8 113.9(4) . . ?
C9 C8 C13 119.0(5) . . ?
C9 C8 C7 119.3(5) . . ?
C13 C8 C7 121.7(4) . . ?
C8 C9 C10 120.0(6) . . ?
C11 C10 C9 119.3(5) . . ?
C11 C10 C19 119.6(6) . . ?
C9 C10 C19 121.0(6) . . ?
C12 C11 C10 121.8(6) . . ?
C11 C12 C13 116.7(5) . . ?
C11 C12 C20 119.1(5) . . ?
C13 C12 C20 124.2(5) . . ?
C8 C13 C12 122.6(5) . . ?
C8 C13 O2 117.9(5) . . ?
C12 C13 O2 119.4(5) . . ?
C17 C14 C15 108.9(6) . . ?
C17 C14 C16 108.7(6) . . ?
C15 C14 C16 105.3(5) . . ?
C17 C14 C2 109.4(5) . . ?
C15 C14 C2 113.0(5) . . ?
C16 C14 C2 111.3(5) . . ?
C23 C20 C21 109.3(6) . . ?
C23 C20 C22 109.1(6) . . ?
C21 C20 C22 106.9(6) . . ?
C23 C20 C12 109.3(5) . . ?
C21 C20 C12 111.3(5) . . ?
C22 C20 C12 110.9(5) . . ?
C25 C24 O3 126.2(4) . . ?
C25 C24 C29 123.8(5) . . ?
O3 C24 C29 109.9(4) . . ?
C24 C25 C26 117.5(5) . . ?
C24 C25 Cl1 120.8(4) . . ?
C26 C25 Cl1 121.6(4) . . ?
C27 C26 C25 119.9(5) . . ?
C27 C26 Cl2 119.9(4) . . ?
C25 C26 Cl2 120.2(4) . . ?
C26 C27 C28 121.1(4) . . ?
C26 C27 Cl3 119.9(4) . . ?
C28 C27 Cl3 119.0(4) . . ?
C29 C28 C27 117.9(5) . . ?
C29 C28 Cl4 118.6(4) . . ?
C27 C28 Cl4 123.5(4) . . ?
O4 C29 C24 113.0(4) . . ?
O4 C29 C28 127.2(4) . . ?
C24 C29 C28 119.8(4) . . ?
C32 C31 C36 120.8(8) . . ?
C32 C31 N 121.3(8) . . ?
C36 C31 N 117.3(7) . . ?
C31 C32 C33 120.8(13) . . ?
C34 C33 C32 122.5(17) . . ?
C33 C34 C35 120.9(11) . . ?
C36 C35 C34 116.0(12) . . ?
C35 C36 C31 118.9(11) . . ?
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 O2 1.595(4) . ?
P O1 1.607(4) . ?
P O3 1.661(4) . ?
P N 1.727(4) . ?
P O4 1.769(3) . ?
Cl1 C25 1.712(5) . ?
Cl2 C26 1.724(5) . ?
Cl3 C27 1.716(5) . ?
Cl4 C28 1.710(5) . ?
O1 C1 1.415(6) . ?
O2 C13 1.414(6) . ?
O3 C24 1.372(6) . ?
O4 C29 1.325(6) . ?
N C31 1.426(7) . ?
N C30 1.442(8) . ?
C1 C6 1.387(7) . ?
C1 C2 1.393(7) . ?
C2 C3 1.387(7) . ?
C2 C14 1.543(7) . ?
C3 C4 1.395(8) . ?
C4 C5 1.390(8) . ?
C4 C18 1.502(8) . ?
C5 C6 1.384(7) . ?
C6 C7 1.513(7) . ?
C7 C8 1.528(8) . ?
C8 C9 1.366(7) . ?
C8 C13 1.389(7) . ?
C9 C10 1.409(9) . ?
C10 C11 1.389(9) . ?
C10 C19 1.536(8) . ?
C11 C12 1.382(8) . ?
C12 C13 1.399(7) . ?
C12 C20 1.568(8) . ?
C14 C17 1.513(8) . ?
C14 C15 1.517(8) . ?
C14 C16 1.537(8) . ?
C20 C23 1.509(8) . ?
C20 C21 1.523(9) . ?
C20 C22 1.539(9) . ?
C24 C25 1.361(7) . ?
C24 C29 1.377(7) . ?
C25 C26 1.408(7) . ?
C26 C27 1.395(7) . ?
C27 C28 1.410(7) . ?
C28 C29 1.388(6) . ?
C31 C32 1.361(10) . ?
C31 C36 1.409(12) . ?
C32 C33 1.380(15) . ?
C33 C34 1.26(3) . ?
C34 C35 1.52(2) . ?
C35 C36 1.408(12) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661053
