#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027500.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027500
loop_
_publ_author_name
'Mitzel, Norbert W.'
'Lustig, Christian'
_publ_section_title
;
 The molecular and crystal structures of the
 tris(dimethylamino)phosphoranes (Me2N)3P--X (X = BH3, CH2,
 NH or O)
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3177
_journal_paper_doi               10.1039/a903292d
_journal_year                    1999
_chemical_compound_source        Fluka
_chemical_formula_sum            'C6 H19 N4 P'
_chemical_formula_weight         178.22
_chemical_melting_point          254.15
_chemical_name_systematic
; 
 Tris(dimethylamino)iminophosphorane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.512(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2190(9)
_cell_length_b                   10.0901(3)
_cell_length_c                   12.1644(14)
_cell_measurement_reflns_used    88
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1000.14(16)
_computing_cell_refinement       'CAD4 Software'
_computing_data_collection       'CAD4 Software'
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_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  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2863
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       Column
_exptl_crystal_F_000             392
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0714P)²+0.2105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1054
_refine_ls_wR_factor_obs         0.1006
_reflns_number_observed          1995
_reflns_number_total             2177
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903292Dsup1.cif
_cod_data_source_block           mit7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-19' was changed to '254.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.2105P] 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^)+(0.0714P)^2^+0.2105P] 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        1000.1(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027500
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
P 0.0278(2) 0.0136(2) 0.0304(2) -0.00194(10) 0.00792(14) -0.00261(10)
N1 0.0295(6) 0.0210(5) 0.0327(6) -0.0051(4) 0.0067(4) -0.0013(4)
N2 0.0341(6) 0.0207(5) 0.0348(6) -0.0071(4) 0.0125(5) -0.0062(4)
N3 0.0312(6) 0.0205(5) 0.0373(6) 0.0001(4) 0.0088(4) 0.0024(4)
N4 0.0402(6) 0.0206(6) 0.0444(7) 0.0027(5) 0.0089(5) -0.0090(5)
C11 0.0362(8) 0.0364(8) 0.0520(9) -0.0097(7) -0.0025(7) 0.0054(6)
C12 0.0411(8) 0.0277(7) 0.0315(6) -0.0075(5) 0.0078(6) -0.0046(6)
C21 0.0401(7) 0.0205(6) 0.0337(7) -0.0058(5) 0.0065(6) 0.0011(5)
C22 0.0421(8) 0.0293(7) 0.0445(8) -0.0070(6) 0.0208(7) -0.0104(6)
C31 0.0330(7) 0.0424(9) 0.0541(9) -0.0025(7) 0.0143(7) 0.0069(6)
C32 0.0514(9) 0.0216(7) 0.0486(9) 0.0067(6) 0.0093(7) 0.0064(6)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
P P 0.04761(4) 0.16135(3) 0.83076(3) 0.02356(14) Uani 1 d
N1 N 0.19557(13) 0.22424(11) 0.92425(9) 0.0275(3) Uani 1 d
N2 N 0.15077(14) 0.14743(10) 0.72281(10) 0.0292(3) Uani 1 d
N3 N -0.09294(14) 0.27823(11) 0.80512(10) 0.0293(3) Uani 1 d
N4 N -0.0441(2) 0.03262(12) 0.85743(11) 0.0348(3) Uani 1 d
C11 C 0.3371(2) 0.1371(2) 0.9561(2) 0.0422(4) Uani 1 d
C12 C 0.1416(2) 0.28887(14) 1.02118(12) 0.0332(3) Uani 1 d
C21 C 0.0903(2) 0.05785(13) 0.63297(12) 0.0313(3) Uani 1 d
C22 C 0.2748(2) 0.2389(2) 0.69325(14) 0.0373(3) Uani 1 d
C31 C -0.2473(2) 0.2740(2) 0.8520(2) 0.0424(4) Uani 1 d
C32 C -0.0526(2) 0.40972(15) 0.76813(14) 0.0403(4) Uani 1 d
H1 H 0.0076(28) -0.0160(26) 0.8959(18) 0.062(7) Uiso 1 d
H11A H 0.3074(26) 0.0629(23) 1.0097(18) 0.057(6) Uiso 1 d
H11B H 0.4300(28) 0.1897(24) 0.9942(20) 0.066(6) Uiso 1 d
H11C H 0.3793(24) 0.0996(21) 0.8885(16) 0.048(5) Uiso 1 d
H12A H 0.1140(25) 0.2258(24) 1.0791(17) 0.058(6) Uiso 1 d
H12B H 0.0513(24) 0.3497(19) 0.9997(16) 0.042(5) Uiso 1 d
H12C H 0.2293(25) 0.3436(20) 1.0581(17) 0.051(6) Uiso 1 d
H21A H 0.1813(21) 0.0041(20) 0.6132(14) 0.038(4) Uiso 1 d
H21B H 0.0440(24) 0.1007(22) 0.5657(17) 0.051(5) Uiso 1 d
H21C H 0.0097(22) 0.0059(18) 0.6542(13) 0.034(4) Uiso 1 d
H22A H 0.3661(24) 0.1923(20) 0.6762(16) 0.044(5) Uiso 1 d
H22B H 0.3068(23) 0.2980(21) 0.7513(17) 0.048(5) Uiso 1 d
H22B H 0.2338(24) 0.2852(22) 0.6285(17) 0.048(5) Uiso 1 d
H31A H -0.2754(26) 0.1828(24) 0.8712(18) 0.057(6) Uiso 1 d
H31B H -0.3325(26) 0.3042(22) 0.8027(17) 0.052(5) Uiso 1 d
H31C H -0.2442(24) 0.3302(20) 0.9175(18) 0.050(6) Uiso 1 d
H32A H 0.0386(25) 0.4067(21) 0.7251(16) 0.049(5) Uiso 1 d
H32B H -0.0295(28) 0.4730(23) 0.8298(19) 0.060(6) Uiso 1 d
H32C H -0.1415(26) 0.4486(22) 0.7259(17) 0.051(5) Uiso 1 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'
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
N4 P N3 106.80(7)
N4 P N2 113.94(6)
N3 P N2 109.15(6)
N4 P N1 120.15(7)
N3 P N1 106.56(6)
N2 P N1 99.69(6)
C12 N1 C11 111.51(12)
C12 N1 P 116.42(9)
C11 N1 P 115.55(9)
C21 N2 C22 112.96(11)
C21 N2 P 119.17(9)
C22 N2 P 126.08(9)
C32 N3 C31 113.17(12)
C32 N3 P 121.86(10)
C31 N3 P 121.87(10)
P N4 H1 114.5(18)
N1 C11 H11A 110.7(12)
N1 C11 H11B 109.7(14)
H11A C11 H11B 108.7(18)
N1 C11 H11C 110.8(11)
H11A C11 H11C 112.0(17)
H11B C11 H11C 104.9(17)
N1 C12 H12A 113.9(13)
N1 C12 H12B 111.4(11)
H12A C12 H12B 110.9(16)
N1 C12 H12C 109.9(12)
H12A C12 H12C 105.1(16)
H12B C12 H12C 105.1(16)
N2 C21 H21A 109.4(10)
N2 C21 H21B 114.8(13)
H21A C21 H21B 105.7(15)
N2 C21 H21C 109.6(10)
H21A C21 H21C 111.1(16)
H21B C21 H21C 106.2(16)
N2 C22 H22A 110.2(12)
N2 C22 H22B 110.8(12)
H22A C22 H22B 109.5(16)
N2 C22 H22B 109.7(12)
H22A C22 H22B 106.0(16)
H22B C22 H22B 110.6(18)
N3 C31 H31A 111.3(13)
N3 C31 H31B 111.4(13)
H31A C31 H31B 106.5(19)
N3 C31 H31C 111.8(12)
H31A C31 H31C 109.4(18)
H31B C31 H31C 106.2(18)
N3 C32 H32A 111.3(12)
N3 C32 H32B 112.7(13)
H32A C32 H32B 110.2(19)
N3 C32 H32C 111.3(13)
H32A C32 H32C 108.9(17)
H32B C32 H32C 102.0(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P N4 1.5572(12)
P N3 1.6518(11)
P N2 1.6594(11)
P N1 1.6773(11)
N1 C12 1.466(2)
N1 C11 1.469(2)
N2 C21 1.455(2)
N2 C22 1.455(2)
N3 C32 1.453(2)
N3 C31 1.458(2)
N4 H1 0.77(2)
C11 H11A 1.04(2)
C11 H11B 0.99(2)
C11 H11C 1.01(2)
C12 H12A 1.00(2)
C12 H12B 0.97(2)
C12 H12C 0.97(2)
C21 H21A 0.98(2)
C21 H21B 0.96(2)
C21 H21C 0.91(2)
C22 H22A 0.93(2)
C22 H22B 0.94(2)
C22 H22B 0.94(2)
C31 H31A 0.98(2)
C31 H31B 0.91(2)
C31 H31C 0.97(2)
C32 H32A 0.97(2)
C32 H32B 0.98(2)
C32 H32C 0.92(2)
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
N4 P N1 C12 -73.06(12)
N3 P N1 C12 48.37(11)
N2 P N1 C12 161.83(10)
N4 P N1 C11 60.67(13)
N3 P N1 C11 -177.90(11)
N2 P N1 C11 -64.45(12)
N4 P N2 C21 30.65(13)
N3 P N2 C21 -88.62(11)
N1 P N2 C21 159.94(11)
N4 P N2 C22 -165.73(13)
N3 P N2 C22 75.00(14)
N1 P N2 C22 -36.44(14)
N4 P N3 C32 -174.88(12)
N2 P N3 C32 -51.28(13)
N1 P N3 C32 55.54(13)
N4 P N3 C31 26.38(14)
N2 P N3 C31 149.99(12)
N1 P N3 C31 -103.20(12)
