#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/08/4310810.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_4310810
loop_
_publ_author_name
'Pavel Rovnaník'
'Libor Kapička'
'Jan Taraba'
'Miloš Černík'
_publ_section_title
;
 Base-Induced Dismutation of POCl3 and POBr3: Synthesis and Structure of
 Ligand-Stabilized Dioxophosphonium Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2435
_journal_page_last               2442
_journal_paper_doi               10.1021/ic0354163
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C16 H23 Cl N5 O2 P'
_chemical_formula_weight         383.81
_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                89.47(3)
_cell_angle_beta                 82.93(3)
_cell_angle_gamma                89.03(3)
_cell_formula_units_Z            2
_cell_length_a                   8.910(2)
_cell_length_b                   10.128(2)
_cell_length_c                   10.282(2)
_cell_measurement_reflns_used    5133
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.695
_cell_measurement_theta_min      0.020
_cell_volume                     920.6(3)
_computing_cell_refinement       'KUMA KM-4 software'
_computing_data_collection       'KUMA KM-4 Crysalis V170'
_computing_data_reduction        'KUMA KM-4 software'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Kuma KM-4 CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6855
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        'not applicable'
_diffrn_standards_interval_count 'not applicable'
_diffrn_standards_interval_time  'not applicable'
_diffrn_standards_number         'not applicable'
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SHELXTL
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nedle
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0302
_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)+(0.0412P)²+0.2659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                3430
_reflns_number_total             3968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354163si20031209_110655_1.cif
_cod_data_source_block           pcld2a
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.2659P] 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^)+(0.0412P)^2^+0.2659P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310810
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
P1 P 0.28896(4) 0.62835(3) 0.31612(3) 0.01636(10) Uani 1 d . . .
O1 O 0.43212(12) 0.55414(10) 0.31354(10) 0.0222(2) Uani 1 d . . .
O2 O 0.15005(12) 0.60788(10) 0.40515(10) 0.0226(2) Uani 1 d . . .
Cl1 Cl 0.09471(4) 1.04812(4) -0.25877(4) 0.02552(10) Uani 1 d . . .
N1 N 0.24183(13) 0.62235(11) 0.15449(11) 0.0152(2) Uani 1 d . . .
C1 C 0.30802(15) 0.52869(13) 0.07076(14) 0.0172(3) Uani 1 d . . .
H1 H 0.3844 0.4750 0.0976 0.021 Uiso 1 d R . .
C2 C 0.26616(16) 0.51116(14) -0.05050(14) 0.0180(3) Uani 1 d . . .
H2 H 0.3118 0.4445 -0.1039 0.022 Uiso 1 d R . .
C3 C 0.15313(15) 0.59394(13) -0.09635(13) 0.0153(3) Uani 1 d . . .
C4 C 0.08735(15) 0.69200(13) -0.00735(14) 0.0172(3) Uani 1 d . . .
H4 H 0.0141 0.7500 -0.0328 0.021 Uiso 1 d R . .
C5 C 0.13085(15) 0.70143(13) 0.11433(14) 0.0169(3) Uani 1 d . . .
H5 H 0.0834 0.7638 0.1720 0.020 Uiso 1 d R . .
N3 N 0.11145(13) 0.57959(11) -0.21557(11) 0.0171(2) Uani 1 d . . .
C6 C 0.00186(16) 0.67064(15) -0.26541(14) 0.0220(3) Uani 1 d . . .
H6A H -0.0960 0.6585 -0.2167 0.033 Uiso 1 d R . .
H6B H -0.0032 0.6531 -0.3563 0.033 Uiso 1 d R . .
H6C H 0.0330 0.7599 -0.2558 0.033 Uiso 1 d R . .
C7 C 0.17459(16) 0.47135(14) -0.30068(14) 0.0198(3) Uani 1 d . . .
H7A H 0.2826 0.4788 -0.3166 0.030 Uiso 1 d R . .
H7B H 0.1330 0.4763 -0.3824 0.030 Uiso 1 d R . .
H7C H 0.1494 0.3883 -0.2586 0.030 Uiso 1 d R . .
C8 C 0.22986(15) 0.88170(14) 0.39402(13) 0.0166(3) Uani 1 d . . .
H8 H 0.1338 0.8522 0.4254 0.020 Uiso 1 d R . .
C9 C 0.26520(15) 1.00812(14) 0.41578(13) 0.0173(3) Uani 1 d . . .
H9 H 0.1937 1.0636 0.4619 0.021 Uiso 1 d R . .
C10 C 0.41066(15) 1.05728(13) 0.36893(13) 0.0148(3) Uani 1 d . . .
C11 C 0.51289(15) 0.96655(13) 0.29746(13) 0.0164(3) Uani 1 d . . .
H11 H 0.6087 0.9940 0.2625 0.020 Uiso 1 d R . .
C12 C 0.47122(15) 0.84110(13) 0.28032(13) 0.0164(3) Uani 1 d . . .
H12 H 0.5405 0.7833 0.2348 0.020 Uiso 1 d R . .
N2 N 0.33082(12) 0.79551(11) 0.32726(11) 0.0146(2) Uani 1 d . . .
C13 C 0.34267(17) 1.27170(14) 0.46645(15) 0.0225(3) Uani 1 d . . .
H13A H 0.2689 1.3021 0.4119 0.034 Uiso 1 d R . .
H13B H 0.3964 1.3457 0.4941 0.034 Uiso 1 d R . .
H13C H 0.2927 1.2270 0.5420 0.034 Uiso 1 d R . .
C14 C 0.59310(17) 1.23552(15) 0.33320(15) 0.0241(3) Uani 1 d . . .
H14A H 0.6733 1.1724 0.3403 0.036 Uiso 1 d R . .
H14B H 0.6128 1.3149 0.3782 0.036 Uiso 1 d R . .
H14C H 0.5874 1.2555 0.2425 0.036 Uiso 1 d R . .
N5 N 0.42172(19) 1.22331(14) 0.04639(15) 0.0370(4) Uani 1 d . . .
N4 N 0.44953(13) 1.18047(11) 0.39218(12) 0.0179(2) Uani 1 d . . .
C16 C 0.34568(18) 1.13357(16) 0.04670(15) 0.0253(3) Uani 1 d . . .
C15 C 0.25082(18) 1.01865(17) 0.04418(16) 0.0284(3) Uani 1 d . . .
H15A H 0.2004 1.0217 -0.0331 0.043 Uiso 1 d R . .
H15B H 0.1769 1.0184 0.1205 0.043 Uiso 1 d R . .
H15C H 0.3124 0.9399 0.0436 0.043 Uiso 1 d 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'
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
O2 P1 O1 127.11(7) . . ?
O2 P1 N2 106.03(7) . . ?
O1 P1 N2 107.07(6) . . ?
O2 P1 N1 107.53(6) . . ?
O1 P1 N1 105.45(6) . . ?
N2 P1 N1 100.66(6) . . ?
C5 N1 C1 118.66(12) . . ?
C5 N1 P1 121.58(10) . . ?
C1 N1 P1 119.51(10) . . ?
C2 C1 N1 122.20(13) . . ?
C1 C2 C3 120.48(13) . . ?
N3 C3 C2 121.55(13) . . ?
N3 C3 C4 122.41(12) . . ?
C2 C3 C4 116.04(12) . . ?
C5 C4 C3 120.51(13) . . ?
C4 C5 N1 122.05(13) . . ?
C3 N3 C6 121.24(12) . . ?
C3 N3 C7 120.59(11) . . ?
C6 N3 C7 118.17(11) . . ?
C9 C8 N2 122.17(13) . . ?
C8 C9 C10 120.70(13) . . ?
N4 C10 C9 121.80(13) . . ?
N4 C10 C11 122.05(12) . . ?
C9 C10 C11 116.15(12) . . ?
C12 C11 C10 120.25(13) . . ?
C11 C12 N2 122.61(13) . . ?
C8 N2 C12 118.10(12) . . ?
C8 N2 P1 120.96(10) . . ?
C12 N2 P1 120.63(10) . . ?
C10 N4 C14 121.90(12) . . ?
C10 N4 C13 121.03(12) . . ?
C14 N4 C13 116.73(11) . . ?
N5 C16 C15 178.69(17) . . ?
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
P1 O2 1.4626(12) . ?
P1 O1 1.4671(11) . ?
P1 N2 1.7476(12) . ?
P1 N1 1.7653(12) . ?
N1 C5 1.3628(18) . ?
N1 C1 1.3638(18) . ?
C1 C2 1.3587(19) . ?
C2 C3 1.4214(19) . ?
C3 N3 1.3338(17) . ?
C3 C4 1.426(2) . ?
C4 C5 1.3592(19) . ?
N3 C6 1.4664(18) . ?
N3 C7 1.4696(18) . ?
C8 C9 1.3509(19) . ?
C8 N2 1.3693(18) . ?
C9 C10 1.4225(19) . ?
C10 N4 1.3320(17) . ?
C10 C11 1.426(2) . ?
C11 C12 1.3488(19) . ?
C12 N2 1.3704(17) . ?
C13 N4 1.4655(19) . ?
C14 N4 1.4635(19) . ?
N5 C16 1.142(2) . ?
C16 C15 1.452(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660882
