#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:37:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179980 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/74/7027499.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_7027499
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_formula_sum            'C6 H21 B N3 P'
_chemical_formula_weight         177.04
_chemical_melting_point          292
_chemical_name_systematic
; 
 tris(dimethylamino)phosphane-borane 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 96.29(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.996(2)
_cell_length_b                   11.174(1)
_cell_length_c                   7.679(1)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      22
_cell_volume                     1108.4(2)
_computing_cell_refinement       CAD4-Software
_computing_data_collection       CAD4-Software
_computing_data_reduction        CADSHEL
_computing_molecular_graphics    SHELXTL-5.01
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4672
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        None
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(6)
_refine_ls_extinction_coef       0.0015(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.083
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2398
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.097
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_obs          0.0207
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0361P)²+0.0772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0556
_refine_ls_wR_factor_obs         0.0543
_reflns_number_observed          2335
_reflns_number_total             2399
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903292Dsup1.cif
_cod_data_source_block           lus2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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^)+(0.0361P)^2^+0.0772P] 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^)+(0.0361P)^2^+0.0772P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7027499
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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
P1 P 0.13216(3) 0.76043(2) 0.95610(4) 0.02042(8) Uani 1 d
B1 B 0.11910(11) 0.79390(13) 1.1970(2) 0.0316(3) Uani 1 d
N1 N 0.13427(7) 0.61419(8) 0.90498(11) 0.0251(2) Uani 1 d
N2 N 0.03383(8) 0.81191(10) 0.82300(14) 0.0323(2) Uani 1 d
N3 N 0.24606(7) 0.80345(9) 0.89987(13) 0.0287(2) Uani 1 d
C11 C 0.03555(13) 0.5508(2) 0.9082(2) 0.0396(4) Uani 1 d
C12 C 0.22001(13) 0.54337(15) 0.9907(2) 0.0374(3) Uani 1 d
C21 C -0.04763(11) 0.8860(2) 0.8811(2) 0.0411(3) Uani 1 d
C22 C 0.02615(13) 0.7957(2) 0.6334(2) 0.0449(3) Uani 1 d
C31 C 0.28656(12) 0.91752(13) 0.9696(2) 0.0385(3) Uani 1 d
C32 C 0.28283(13) 0.77184(14) 0.7336(2) 0.0434(3) Uani 1 d
H1A H 0.0439(16) 0.7420(15) 1.2237(27) 0.040(5) Uiso 1 d
H1B H 0.1180(15) 0.8913(18) 1.2187(28) 0.050(5) Uiso 1 d
H1C H 0.1906(19) 0.7563(19) 1.2758(33) 0.051(7) Uiso 1 d
H11A H 0.0459(16) 0.4693(21) 0.8595(29) 0.055(5) Uiso 1 d
H11B H 0.0180(19) 0.5392(24) 1.0074(37) 0.074(7) Uiso 1 d
H11C H -0.0150(15) 0.5948(16) 0.8433(27) 0.036(4) Uiso 1 d
H12A H 0.2795(15) 0.5813(16) 0.9809(24) 0.035(4) Uiso 1 d
H12B H 0.2206(13) 0.4701(18) 0.9357(25) 0.040(4) Uiso 1 d
H12C H 0.2154(15) 0.5236(19) 1.1059(30) 0.048(5) Uiso 1 d
H21A H -0.0367(16) 0.8902(17) 0.9926(29) 0.045(5) Uiso 1 d
H21B H -0.1089(18) 0.8536(20) 0.8469(29) 0.055(5) Uiso 1 d
H21C H -0.0499(15) 0.9608(18) 0.8244(29) 0.051(5) Uiso 1 d
H22A H 0.0408(20) 0.8701(28) 0.5746(37) 0.077(7) Uiso 1 d
H22B H -0.0492(22) 0.7783(23) 0.5853(38) 0.072(7) Uiso 1 d
H22C H 0.0656(24) 0.7339(27) 0.6105(41) 0.074(9) Uiso 1 d
H31A H 0.2602(13) 0.9789(18) 0.8847(27) 0.046(5) Uiso 1 d
H31B H 0.2612(19) 0.9388(22) 1.0841(34) 0.068(7) Uiso 1 d
H31C H 0.3617(16) 0.9140(19) 0.9784(26) 0.052(5) Uiso 1 d
H32A H 0.2546(16) 0.6914(18) 0.6918(29) 0.051(5) Uiso 1 d
H32B H 0.3627(21) 0.7738(22) 0.7592(38) 0.073(7) Uiso 1 d
H32C H 0.2610(15) 0.8288(18) 0.6469(28) 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'
B B 0.0013 0.0007 '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
N2 P1 N3 112.99(6)
N2 P1 N1 103.03(6)
N3 P1 N1 100.55(5)
N2 P1 B1 112.72(6)
N3 P1 B1 111.81(6)
N1 P1 B1 114.90(6)
P1 B1 H1A 103.6(10)
P1 B1 H1B 110.1(11)
H1A B1 H1B 116.0(14)
P1 B1 H1C 106.8(13)
H1A B1 H1C 111.9(15)
H1B B1 H1C 108.0(16)
C12 N1 C11 110.82(11)
C12 N1 P1 116.86(9)
C11 N1 P1 115.36(10)
C21 N2 C22 113.87(12)
C21 N2 P1 123.34(10)
C22 N2 P1 122.58(9)
C32 N3 C31 113.23(11)
C32 N3 P1 123.14(9)
C31 N3 P1 117.02(9)
N1 C11 H11A 106.2(12)
N1 C11 H11B 114.8(18)
H11A C11 H11B 105.2(22)
N1 C11 H11C 107.8(11)
H11A C11 H11C 113.6(17)
H11B C11 H11C 109.3(21)
N1 C12 H12A 109.2(11)
N1 C12 H12B 108.6(12)
H12A C12 H12B 109.4(15)
N1 C12 H12C 115.9(12)
H12A C12 H12C 110.1(17)
H12B C12 H12C 103.4(17)
N2 C21 H21A 107.1(13)
N2 C21 H21B 109.7(14)
H21A C21 H21B 111.4(19)
N2 C21 H21C 110.6(12)
H21A C21 H21C 114.0(19)
H21B C21 H21C 104.1(18)
N2 C22 H22A 111.2(17)
N2 C22 H22B 110.0(15)
H22A C22 H22B 102.8(21)
N2 C22 H22C 108.4(20)
H22A C22 H22C 115.1(24)
H22B C22 H22C 109.2(25)
N3 C31 H31A 106.3(11)
N3 C31 H31B 113.0(14)
H31A C31 H31B 107.0(18)
N3 C31 H31C 108.0(13)
H31A C31 H31C 110.4(16)
H31B C31 H31C 111.9(19)
N3 C32 H32A 110.6(12)
N3 C32 H32B 104.3(16)
H32A C32 H32B 113.6(18)
N3 C32 H32C 110.7(12)
H32A C32 H32C 107.8(18)
H32B C32 H32C 109.8(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N2 1.6499(11)
P1 N3 1.6579(10)
P1 N1 1.6815(9)
P1 B1 1.9133(14)
B1 H1A 1.17(2)
B1 H1B 1.10(2)
B1 H1C 1.13(2)
N1 C12 1.463(2)
N1 C11 1.468(2)
N2 C21 1.452(2)
N2 C22 1.459(2)
N3 C32 1.455(2)
N3 C31 1.458(2)
C11 H11A 1.00(2)
C11 H11B 0.83(3)
C11 H11C 0.92(2)
C12 H12A 0.89(2)
C12 H12B 0.92(2)
C12 H12C 0.92(2)
C21 H21A 0.85(2)
C21 H21B 0.89(2)
C21 H21C 0.94(2)
C22 H22A 0.97(3)
C22 H22B 1.03(3)
C22 H22C 0.89(3)
C31 H31A 0.98(2)
C31 H31B 1.00(3)
C31 H31C 0.97(2)
C32 H32A 1.01(2)
C32 H32B 1.04(3)
C32 H32C 0.94(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
N2 P1 N1 C12 174.67(10)
N3 P1 N1 C12 57.87(10)
B1 P1 N1 C12 -62.34(11)
N2 P1 N1 C11 -52.42(11)
N3 P1 N1 C11 -169.22(10)
B1 P1 N1 C11 70.57(11)
N3 P1 N2 C21 -121.52(12)
N1 P1 N2 C21 130.88(12)
B1 P1 N2 C21 6.44(14)
N3 P1 N2 C22 52.82(13)
N1 P1 N2 C22 -54.77(13)
B1 P1 N2 C22 -179.21(12)
N2 P1 N3 C32 -61.66(12)
N1 P1 N3 C32 47.50(12)
B1 P1 N3 C32 169.90(12)
N2 P1 N3 C31 87.84(11)
N1 P1 N3 C31 -162.99(10)
B1 P1 N3 C31 -40.59(12)
