#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/22/7052229.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_7052229
loop_
_publ_author_name
'Kumar, K. V. P. Pavan'
'Kumar, N. Satish'
'Kumara Swamy, K. C.'
_publ_section_title
;
 Structurally diverse penta- and hexacoordinate phosphorus compounds
 from the reaction of diethyl or diisopropyl azodicarboxylates with
 phosphorus(iii) compounds
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              717
_journal_paper_doi               10.1039/b514839a
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C30 H42 Cl N2 O6 P S'
_chemical_formula_weight         625.14
_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                92.5670(10)
_cell_angle_beta                 103.1120(10)
_cell_angle_gamma                111.9970(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4788(7)
_cell_length_b                   10.8660(7)
_cell_length_c                   16.3413(11)
_cell_measurement_temperature    273(2)
_cell_volume                     1662.80(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16112
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9484
_exptl_absorpt_correction_T_min  0.9240
_exptl_absorpt_correction_type   'EMPIRICAL, SADABS'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'THICK NEEDLES'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0637P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                4167
_reflns_number_total             5836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514839a.txt
_cod_data_source_block           compd16
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      p_-1
_cod_database_code               7052229
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
P P 0.57776(6) 0.66016(6) 0.27176(3) 0.04043(16) Uani 1 1 d . . .
S S 0.51147(6) 0.54219(6) 0.38032(3) 0.04812(17) Uani 1 1 d . . .
Cl Cl 0.77385(6) 0.61959(7) 0.30976(4) 0.06001(19) Uani 1 1 d . . .
O1 O 0.42690(14) 0.68551(13) 0.25266(9) 0.0420(3) Uani 1 1 d . . .
O2 O 0.49516(15) 0.51286(14) 0.20788(8) 0.0450(4) Uani 1 1 d . . .
O3 O 0.62829(15) 0.73530(14) 0.19100(8) 0.0441(4) Uani 1 1 d . . .
O6 O 0.77955(16) 0.97193(16) 0.45234(9) 0.0566(4) Uani 1 1 d . . .
O5 O 0.58201(17) 0.78908(15) 0.44863(9) 0.0538(4) Uani 1 1 d . . .
N1 N 0.67511(18) 0.81836(17) 0.33604(10) 0.0441(4) Uani 1 1 d . . .
O4 O 0.79385(17) 0.90904(16) 0.15910(10) 0.0584(4) Uani 1 1 d . . .
C17 C 0.4885(2) 0.3954(2) 0.23855(13) 0.0442(5) Uani 1 1 d . . .
N2 N 0.76959(19) 0.91020(18) 0.29633(11) 0.0500(5) Uani 1 1 d . . .
C23 C 0.6734(2) 0.8555(2) 0.41569(13) 0.0439(5) Uani 1 1 d . . .
C12 C 0.4949(2) 0.3924(2) 0.32410(13) 0.0454(5) Uani 1 1 d . . .
C1 C 0.3125(2) 0.6054(2) 0.27930(13) 0.0423(5) Uani 1 1 d . . .
C16 C 0.4785(2) 0.2854(2) 0.18682(14) 0.0446(5) Uani 1 1 d . . .
C2 C 0.1759(2) 0.5982(2) 0.24122(14) 0.0461(5) Uani 1 1 d . . .
C15 C 0.4848(2) 0.1776(2) 0.22922(15) 0.0524(6) Uani 1 1 d . . .
H10 H 0.4782 0.1016 0.1971 0.063 Uiso 1 1 calc R . .
C27 C 0.7344(2) 0.8568(2) 0.21937(14) 0.0461(5) Uani 1 1 d . . .
C6 C 0.3353(2) 0.5345(2) 0.34536(13) 0.0457(5) Uani 1 1 d . . .
C18 C 0.4646(3) 0.2825(2) 0.09127(14) 0.0508(6) Uani 1 1 d . . .
C3 C 0.0692(3) 0.5223(2) 0.27770(16) 0.0588(6) Uani 1 1 d . . .
H3 H -0.0228 0.5167 0.2548 0.071 Uiso 1 1 calc R . .
C13 C 0.5030(2) 0.2846(2) 0.36388(15) 0.0533(6) Uani 1 1 d . . .
H8 H 0.5102 0.2856 0.4217 0.064 Uiso 1 1 calc R . .
C7 C 0.1441(2) 0.6648(2) 0.16271(15) 0.0524(6) Uani 1 1 d . . .
C5 C 0.2259(3) 0.4586(2) 0.37905(16) 0.0609(7) Uani 1 1 d . . .
H5 H 0.2434 0.4112 0.4233 0.073 Uiso 1 1 calc R . .
C4 C 0.0916(3) 0.4541(3) 0.34631(18) 0.0659(7) Uani 1 1 d . . .
C14 C 0.5001(3) 0.1762(2) 0.31581(15) 0.0536(6) Uani 1 1 d . . .
C19 C 0.4438(3) 0.1460(3) 0.04847(16) 0.0752(8) Uani 1 1 d . . .
H20A H 0.4344 0.1481 -0.0112 0.113 Uiso 1 1 calc R . .
H20B H 0.3591 0.0783 0.0568 0.113 Uiso 1 1 calc R . .
H20C H 0.5247 0.1257 0.0730 0.113 Uiso 1 1 calc R . .
C28 C 0.9012(3) 1.0467(3) 0.18154(17) 0.0678(7) Uani 1 1 d . . .
H26 H 0.9518 1.0621 0.2418 0.081 Uiso 1 1 calc R . .
C24 C 0.7843(3) 1.0184(3) 0.53881(15) 0.0664(7) Uani 1 1 d . . .
H23 H 0.6866 0.9958 0.5433 0.080 Uiso 1 1 calc R . .
C21 C 0.3338(3) 0.3109(3) 0.04855(15) 0.0678(7) Uani 1 1 d . . .
H22A H 0.3432 0.3962 0.0741 0.102 Uiso 1 1 calc R . .
H22B H 0.2491 0.2418 0.0558 0.102 Uiso 1 1 calc R . .
H22C H 0.3274 0.3123 -0.0109 0.102 Uiso 1 1 calc R . .
C8 C 0.1841(3) 0.6059(3) 0.09047(17) 0.0823(9) Uani 1 1 d . . .
H14A H 0.1636 0.6462 0.0407 0.123 Uiso 1 1 calc R . .
H14B H 0.1297 0.5107 0.0783 0.123 Uiso 1 1 calc R . .
H14C H 0.2840 0.6237 0.1070 0.123 Uiso 1 1 calc R . .
C30 C 0.8311(4) 1.1401(3) 0.1660(3) 0.1220(14) Uani 1 1 d . . .
H28A H 0.7939 1.1347 0.1060 0.183 Uiso 1 1 calc R . .
H28B H 0.8989 1.2297 0.1889 0.183 Uiso 1 1 calc R . .
H28C H 0.7545 1.1172 0.1930 0.183 Uiso 1 1 calc R . .
C26 C 0.8611(4) 1.1680(3) 0.5512(2) 0.1235(15) Uani 1 1 d . . .
H25A H 0.9552 1.1908 0.5439 0.185 Uiso 1 1 calc R . .
H25B H 0.8676 1.2043 0.6073 0.185 Uiso 1 1 calc R . .
H25C H 0.8095 1.2047 0.5101 0.185 Uiso 1 1 calc R . .
C20 C 0.6000(3) 0.3873(3) 0.07719(18) 0.0758(8) Uani 1 1 d . . .
H21A H 0.6112 0.4749 0.0998 0.114 Uiso 1 1 calc R . .
H21B H 0.5931 0.3835 0.0175 0.114 Uiso 1 1 calc R . .
H21C H 0.6809 0.3696 0.1054 0.114 Uiso 1 1 calc R . .
C9 C 0.2298(3) 0.8162(3) 0.1816(2) 0.0807(9) Uani 1 1 d . . .
H15A H 0.3298 0.8346 0.1989 0.121 Uiso 1 1 calc R . .
H15B H 0.2036 0.8534 0.2264 0.121 Uiso 1 1 calc R . .
H15C H 0.2099 0.8560 0.1316 0.121 Uiso 1 1 calc R . .
C22 C 0.5175(3) 0.0591(3) 0.35594(18) 0.0773(8) Uani 1 1 d . . .
H18A H 0.5489 0.0826 0.4166 0.116 Uiso 1 1 calc R . .
H18B H 0.5869 0.0370 0.3362 0.116 Uiso 1 1 calc R . .
H18C H 0.4277 -0.0169 0.3406 0.116 Uiso 1 1 calc R . .
C29 C 1.0023(4) 1.0552(4) 0.1291(3) 0.1428(18) Uani 1 1 d . . .
H27A H 0.9537 1.0431 0.0701 0.214 Uiso 1 1 calc R . .
H27B H 1.0383 0.9864 0.1392 0.214 Uiso 1 1 calc R . .
H27C H 1.0803 1.1415 0.1440 0.214 Uiso 1 1 calc R . .
C11 C -0.0321(3) 0.3751(3) 0.3824(2) 0.1044(12) Uani 1 1 d . . .
H17A H -0.0219 0.2952 0.3996 0.157 Uiso 1 1 calc R . .
H17B H -0.1205 0.3511 0.3397 0.157 Uiso 1 1 calc R . .
H17C H -0.0319 0.4292 0.4306 0.157 Uiso 1 1 calc R . .
C10 C -0.0131(3) 0.6400(3) 0.13196(19) 0.0859(9) Uani 1 1 d . . .
H16A H -0.0277 0.6837 0.0830 0.129 Uiso 1 1 calc R . .
H16B H -0.0418 0.6753 0.1763 0.129 Uiso 1 1 calc R . .
H16C H -0.0691 0.5453 0.1172 0.129 Uiso 1 1 calc R . .
C25 C 0.8542(4) 0.9514(4) 0.60045(18) 0.1052(12) Uani 1 1 d . . .
H24A H 0.8033 0.8560 0.5867 0.158 Uiso 1 1 calc R . .
H24B H 0.8534 0.9798 0.6568 0.158 Uiso 1 1 calc R . .
H24C H 0.9509 0.9754 0.5977 0.158 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'
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'
Cl Cl 0.1484 0.1585 '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
O3 P O1 93.70(7) . . ?
O3 P O2 89.91(7) . . ?
O1 P O2 91.03(7) . . ?
O3 P N1 87.14(7) . . ?
O1 P N1 91.83(8) . . ?
O2 P N1 176.02(8) . . ?
O3 P Cl 92.18(6) . . ?
O1 P Cl 174.03(6) . . ?
O2 P Cl 90.00(6) . . ?
N1 P Cl 87.44(6) . . ?
O3 P S 175.59(6) . . ?
O1 P S 89.24(5) . . ?
O2 P S 86.75(5) . . ?
N1 P S 96.06(6) . . ?
Cl P S 84.95(3) . . ?
C12 S C6 101.13(10) . . ?
C12 S P 91.01(7) . . ?
C6 S P 91.32(7) . . ?
C1 O1 P 121.18(13) . . ?
C17 O2 P 120.90(12) . . ?
C27 O3 P 110.69(13) . . ?
C23 O6 C24 115.86(18) . . ?
C23 N1 N2 119.54(17) . . ?
C23 N1 P 128.31(15) . . ?
N2 N1 P 112.06(13) . . ?
C27 O4 C28 116.32(18) . . ?
O2 C17 C12 116.93(19) . . ?
O2 C17 C16 121.73(19) . . ?
C12 C17 C16 121.3(2) . . ?
C27 N2 N1 105.86(17) . . ?
O5 C23 O6 124.57(19) . . ?
O5 C23 N1 122.5(2) . . ?
O6 C23 N1 112.90(19) . . ?
C13 C12 C17 122.1(2) . . ?
C13 C12 S 122.53(17) . . ?
C17 C12 S 115.04(16) . . ?
O1 C1 C6 118.82(19) . . ?
O1 C1 C2 120.20(19) . . ?
C6 C1 C2 121.0(2) . . ?
C17 C16 C15 114.7(2) . . ?
C17 C16 C18 122.89(19) . . ?
C15 C16 C18 122.4(2) . . ?
C3 C2 C1 115.4(2) . . ?
C3 C2 C7 122.1(2) . . ?
C1 C2 C7 122.45(19) . . ?
C14 C15 C16 124.7(2) . . ?
N2 C27 O4 126.3(2) . . ?
N2 C27 O3 121.5(2) . . ?
O4 C27 O3 112.20(18) . . ?
C1 C6 C5 121.8(2) . . ?
C1 C6 S 115.43(16) . . ?
C5 C6 S 122.73(19) . . ?
C20 C18 C19 108.1(2) . . ?
C20 C18 C16 109.2(2) . . ?
C19 C18 C16 112.10(19) . . ?
C20 C18 C21 110.5(2) . . ?
C19 C18 C21 107.2(2) . . ?
C16 C18 C21 109.68(18) . . ?
C2 C3 C4 124.3(2) . . ?
C14 C13 C12 118.3(2) . . ?
C10 C7 C9 107.9(2) . . ?
C10 C7 C8 107.5(2) . . ?
C9 C7 C8 109.5(2) . . ?
C10 C7 C2 112.5(2) . . ?
C9 C7 C2 110.66(19) . . ?
C8 C7 C2 108.7(2) . . ?
C4 C5 C6 119.1(2) . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 C11 121.4(3) . . ?
C3 C4 C11 120.2(3) . . ?
C13 C14 C15 118.7(2) . . ?
C13 C14 C22 121.1(2) . . ?
C15 C14 C22 120.2(2) . . ?
C30 C28 O4 109.4(2) . . ?
C30 C28 C29 114.1(3) . . ?
O4 C28 C29 105.1(2) . . ?
O6 C24 C25 110.1(2) . . ?
O6 C24 C26 105.8(2) . . ?
C25 C24 C26 113.8(3) . . ?
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 O3 1.6668(14) . ?
P O1 1.6681(14) . ?
P O2 1.6743(14) . ?
P N1 1.7713(17) . ?
P Cl 2.2194(8) . ?
P S 2.3170(8) . ?
S C12 1.762(2) . ?
S C6 1.773(2) . ?
O1 C1 1.369(2) . ?
O2 C17 1.376(2) . ?
O3 C27 1.344(2) . ?
O6 C23 1.331(2) . ?
O6 C24 1.462(3) . ?
O5 C23 1.216(2) . ?
N1 C23 1.352(3) . ?
N1 N2 1.416(2) . ?
O4 C27 1.320(3) . ?
O4 C28 1.463(3) . ?
C17 C12 1.387(3) . ?
C17 C16 1.389(3) . ?
N2 C27 1.272(3) . ?
C12 C13 1.385(3) . ?
C1 C6 1.383(3) . ?
C1 C2 1.396(3) . ?
C16 C15 1.402(3) . ?
C16 C18 1.533(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.533(3) . ?
C15 C14 1.389(3) . ?
C6 C5 1.385(3) . ?
C18 C20 1.524(3) . ?
C18 C19 1.528(3) . ?
C18 C21 1.537(3) . ?
C3 C4 1.395(4) . ?
C13 C14 1.373(3) . ?
C7 C10 1.523(3) . ?
C7 C9 1.527(3) . ?
C7 C8 1.528(3) . ?
C5 C4 1.369(4) . ?
C4 C11 1.524(3) . ?
C14 C22 1.509(3) . ?
C28 C30 1.459(4) . ?
C28 C29 1.488(4) . ?
C24 C25 1.486(4) . ?
C24 C26 1.500(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21141780
