#------------------------------------------------------------------------------
#$Date: 2016-02-13 13:50:18 +0100 (Sat 13 de Feb de 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/35/4123586.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_4123586
loop_
_publ_author_name
'Britvin, Sergey N.'
'Lotnyk, Andriy'
_publ_section_title
;
 Water-Soluble Phosphine Capable of Dissolving Elemental Gold: The Missing
 Link between 1,3,5-Triaza-7-phosphaadamantane (PTA) and Verkade's
 Ephemeral Ligand.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5526
_journal_page_last               5535
_journal_paper_doi               10.1021/jacs.5b01851
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C6 H12 N3 P'
_chemical_formula_sum            'C6 H12 N3 P'
_chemical_formula_weight         157.16
_chemical_name_common            PTA
_chemical_name_systematic        1,3,5-triaza-7-phosphaadamantane
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.4937(1)
_cell_length_b                   9.4937(1)
_cell_length_c                   6.9591(2)
_cell_measurement_reflns_used    6700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.422
_cell_measurement_theta_min      3.620
_cell_volume                     543.194(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 v1.2-ac2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0052
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7935
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         37.50
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    0.301
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         730
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+0.0284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                726
_reflns_number_total             730
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details
;
TITL PTA in R3m
CELL 0.71073 9.4937 9.4937 6.9591 90 90 120
ZERR 3 0.0001 0.0001 0.0002 0 0 0
LATT -3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -Y,-X,+Z
SYMM +Y-X,+Y,+Z
SYMM +X,+X-Y,+Z
 
SFAC C H N P
UNIT 18 36 9 3
 
L.S. 20
PLAN  25
REM R3m (#160 in standard setting)
bond $H
conf
fmap 2
acta
MERG 2
OMIT -4 75

 
WGHT    0.035100    0.028400
FVAR       9.49395
P1    4    0.666667    0.333333    0.503530    10.16667    0.02329    0.02329 =
         0.00883    0.00000    0.00000    0.01165
C1    1    0.569426    0.430574    0.641782    10.50000    0.01539    0.01539 =
         0.01936    0.00314   -0.00314    0.00887
C2    1    0.499773    0.249886    0.915368    10.50000    0.01221    0.01400 =
         0.01705    0.00267    0.00534    0.00611
AFIX  23
H2B   2    0.388890    0.194446    0.867754    10.50000   -1.20000
H2A   2    0.494871    0.247435    1.054634    10.50000   -1.20000
AFIX   0
N1    3    0.580049    0.419951    0.851827    10.50000    0.01122    0.01122 =
         0.01678   -0.00095    0.00095    0.00594
H1    2    0.627930    0.545130    0.606185    11.00000    0.02764
HKLF 4
 
REM  PTA in R3m
REM R1 =  0.0163 for    726 Fo > 4sig(Fo)  and  0.0165 for all    730 data
REM     26 parameters refined using      1 restraints
 
END  
     
WGHT      0.0351      0.0284 
REM Highest difference peak  0.246,  deepest hole -0.165,  1-sigma level  0.039
Q1    1   0.5432  0.3491  0.8789  11.00000  0.05    0.25
Q2    1   0.5749  0.4251  0.7620  10.50000  0.05    0.20
Q3    1   0.6111  0.3889  0.5810  10.50000  0.05    0.19
Q4    1   0.5431  0.4569  0.8731  10.50000  0.05    0.16
Q5    1   0.6667  0.3333  0.3879  10.16667  0.05    0.15
Q6    1   0.6667  0.3333  0.5972  10.16667  0.05    0.14
Q7    1   0.5237  0.3104  1.1220  11.00000  0.05    0.14
Q8    1   0.5870  0.4962  0.5951  11.00000  0.05    0.09
Q9    1   0.3554  0.1777  0.8201  10.50000  0.05    0.09
Q10   1   0.5616  0.2808  0.3946  10.50000  0.05    0.09
Q11   1   0.3016  0.1508  0.7254  10.50000  0.05    0.08
Q12   1   0.5444  0.2722  1.2744  10.50000  0.05    0.08
Q13   1   0.4680  0.2340  1.2258  10.50000  0.05    0.08
Q14   1   0.3325  0.0818  0.9338  11.00000  0.05    0.07
Q15   1   0.2035  0.1017  0.9755  10.50000  0.05    0.06
Q16   1   0.5166  0.4834  0.9476  10.50000  0.05    0.06
Q17   1   0.2312  0.0405  0.8616  11.00000  0.05    0.06
Q18   1   0.4252  0.2126  1.1155  10.50000  0.05    0.06
Q19   1   0.4424  0.1071  1.1321  11.00000  0.05    0.06
Q20   1   0.2127  0.1809  0.9235  11.00000  0.05    0.05
Q21   1   0.5149  0.6124  0.7210  11.00000  0.05    0.05
Q22   1   0.5766  0.1531  0.4086  10.50000  0.05    0.05
Q23   1   0.6205  0.5312  0.8708  11.00000  0.05    0.05
Q24   1   0.6373  0.2746  0.2739  10.50000  0.05    0.05
Q25   1   0.6018  0.5558  0.9116  11.00000  0.05    0.04

;
_cod_data_source_file            PTA.cif
_cod_data_source_block           PTA
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4123579--4123586.cif.
;
_cod_original_cell_volume        543.19(2)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4123586
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
P1 P 0.6667 0.3333 0.503530(16) 0.01847(7) Uani 1 6 d S
C1 C 0.56943(4) 0.43057(4) 0.64178(11) 0.01620(10) Uani 1 2 d S
C2 C 0.49977(7) 0.24989(4) 0.91537(11) 0.01462(10) Uani 1 2 d S
H2B H 0.3889 0.1944 0.8678 0.018 Uiso 1 2 calc SR
H2A H 0.4949 0.2474 1.0546 0.018 Uiso 1 2 calc SR
N1 N 0.58005(3) 0.41995(3) 0.85183(8) 0.01293(9) Uani 1 2 d S
H1 H 0.6279(12) 0.5451(16) 0.6062(17) 0.028(2) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.02329(10) 0.02329(10) 0.00883(9) 0.000 0.000 0.01165(5)
C1 0.01539(16) 0.01539(16) 0.0194(3) 0.00314(9) -0.00314(9) 0.00887(19)
C2 0.0122(2) 0.01400(15) 0.0170(2) 0.00267(8) 0.00534(16) 0.00611(10)
N1 0.01122(13) 0.01122(13) 0.01678(19) -0.00095(7) 0.00095(7) 0.00594(14)
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'
P P 0.1023 0.0942 '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
C1 P1 C1 95.81(3) 2_655 3_665
C1 P1 C1 95.81(3) 2_655 .
C1 P1 C1 95.81(3) 3_665 .
N1 C1 P1 114.22(4) . .
N1 C1 H1 108.0(7) . .
P1 C1 H1 105.9(7) . .
N1 C2 N1 114.43(5) . 2_655
N1 C2 H2B 108.7 . .
N1 C2 H2B 108.7 2_655 .
N1 C2 H2A 108.7 . .
N1 C2 H2A 108.7 2_655 .
H2B C2 H2A 107.6 . .
C2 N1 C2 108.18(6) . 3_665
C2 N1 C1 111.04(4) . .
C2 N1 C1 111.04(4) 3_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C1 1.8661(7) 2_655
P1 C1 1.8662(7) 3_665
P1 C1 1.8661(7) .
C1 N1 1.4721(10) .
C1 H1 0.974(12) .
C2 N1 1.4672(5) .
C2 N1 1.4672(5) 2_655
C2 H2B 0.9700 .
C2 H2A 0.9700 .
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
_geom_torsion_site_symmetry_4
C1 P1 C1 N1 48.236(17) 2_655 .
C1 P1 C1 N1 -48.235(17) 3_665 .
N1 C2 N1 C2 -55.27(10) 2_655 3_665
N1 C2 N1 C1 66.81(7) 2_655 .
P1 C1 N1 C2 -60.20(3) . .
P1 C1 N1 C2 60.20(3) . 3_665
