#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:53:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179429 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/26/4332629.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_4332629
loop_
_publ_author_name
'Wong, Gene W.'
'Harkreader, Jennifer L.'
'Mebi, Charles A.'
'Frost, Brian J.'
_publ_section_title
;
 Synthesis and Coordination Chemistry of a Novel Bidentate
 Phosphine:  6-(Diphenylphosphino)-1,3,5-triaza-7-phosphaadamantane
 (PTA-PPh2)
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6748
_journal_page_last               6755
_journal_paper_doi               10.1021/ic060576a
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C28 H27 N3 O4 P2 W'
_chemical_formula_weight         715.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 110.847(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.015(2)
_cell_length_b                   12.534(3)
_cell_length_c                   11.605(2)
_cell_measurement_reflns_used    5589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.95
_cell_measurement_theta_min      2.31
_cell_volume                     1361.4(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14622
_diffrn_reflns_theta_full        32.37
_diffrn_reflns_theta_max         32.37
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    4.400
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Pale
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.424
_refine_diff_density_min         -2.146
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0387
_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)+(0.0334P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                4161
_reflns_number_total             5022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060576asup4.cif
_cod_data_source_block           bjf146
_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.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4332629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
W1 W 0.95751(2) 0.2500 0.629963(18) 0.01015(6) Uani 1 2 d S
P1 P 0.84853(13) 0.2500 0.39942(11) 0.0116(2) Uani 1 2 d S
P2 P 0.73640(13) 0.2500 0.68524(11) 0.0089(2) Uani 1 2 d S
O1 O 1.1458(4) 0.2500 0.9129(3) 0.0234(8) Uani 1 2 d S
O2 O 1.2637(4) 0.2500 0.6116(4) 0.0358(12) Uani 1 2 d S
O3 O 0.9163(4) 0.0003(2) 0.5889(3) 0.0297(7) Uani 1 1 d .
N1 N 0.6996(3) 0.3483(3) 0.1767(3) 0.0195(7) Uani 1 1 d .
N3 N 0.9167(5) 0.2500 0.1865(4) 0.0143(8) Uani 1 2 d S
C1 C 1.0726(6) 0.2500 0.8100(5) 0.0161(10) Uani 1 2 d S
C2 C 1.1497(6) 0.2500 0.6118(5) 0.0200(11) Uani 1 2 d S
C3 C 0.9374(4) 0.0896(3) 0.6095(3) 0.0184(8) Uani 1 1 d .
C5 C 0.7377(4) 0.3609(3) 0.3113(3) 0.0187(8) Uani 1 1 d .
H5A H 0.7899 0.4286 0.3381 0.027(12) Uiso 1 1 d R
H5B H 0.6490 0.3648 0.3302 0.025(12) Uiso 1 1 d R
C7 C 0.9818(5) 0.2500 0.3222(4) 0.0146(9) Uani 1 2 d S
H7A H 1.0433 0.1863 0.3488 0.025(12) Uiso 1 1 d R
C8 C 0.6170(6) 0.2500 0.1320(5) 0.0230(12) Uani 1 2 d S
H8A H 0.5341 0.2500 0.1593 0.004(12) Uiso 1 2 d SR
H8B H 0.5798 0.2500 0.0409 0.06(2) Uiso 1 2 d SR
C9 C 0.8277(4) 0.3445(3) 0.1419(3) 0.0185(7) Uani 1 1 d .
H9A H 0.7965 0.3459 0.0509 0.021(11) Uiso 1 1 d R
H9B H 0.8862 0.4090 0.1735 0.014(10) Uiso 1 1 d R
C11 C 0.5701(5) 0.2500 0.5524(4) 0.0106(9) Uani 1 2 d S
C12 C 0.5095(4) 0.3455(3) 0.4960(3) 0.0151(7) Uani 1 1 d .
H12A H 0.5510 0.4111 0.5319 0.025(12) Uiso 1 1 d R
C13 C 0.3903(4) 0.3457(3) 0.3874(3) 0.0173(7) Uani 1 1 d .
H13A H 0.3492 0.4117 0.3525 0.037(14) Uiso 1 1 d R
C14 C 0.3306(5) 0.2500 0.3319(4) 0.0163(10) Uani 1 2 d S
H14A H 0.2520 0.2500 0.2563 0.025(17) Uiso 1 2 d SR
C17 C 0.7126(4) 0.1352(3) 0.7758(3) 0.0111(6) Uani 1 1 d .
C18 C 0.5808(4) 0.1147(3) 0.7879(3) 0.0134(6) Uani 1 1 d .
H18A H 0.5017 0.1599 0.7483 0.006(9) Uiso 1 1 d R
C19 C 0.5641(4) 0.0282(3) 0.8569(3) 0.0168(7) Uani 1 1 d .
H19A H 0.4747 0.0158 0.8657 0.020(11) Uiso 1 1 d R
C20 C 0.6783(4) -0.0400(3) 0.9136(3) 0.0173(7) Uani 1 1 d .
H20A H 0.6672 -0.0991 0.9605 0.039(14) Uiso 1 1 d R
C21 C 0.8086(4) -0.0211(3) 0.9016(3) 0.0172(7) Uani 1 1 d .
H21A H 0.8865 -0.0675 0.9401 0.005(9) Uiso 1 1 d R
C22 C 0.8267(4) 0.0668(3) 0.8336(3) 0.0125(6) Uani 1 1 d .
H22A H 0.9169 0.0792 0.8266 0.017(11) Uiso 1 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'
W W -0.8490 6.8722 '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 W1 C2 83.8(2) . .
C1 W1 C3 96.85(10) . .
C2 W1 C3 92.68(10) . .
C1 W1 C3 96.85(10) . 4_565
C2 W1 C3 92.68(10) . 4_565
C3 W1 C3 165.8(2) . 4_565
C1 W1 P1 171.36(15) . .
C2 W1 P1 87.57(15) . .
C3 W1 P1 83.53(10) . .
C3 W1 P1 83.52(10) 4_565 .
C1 W1 P2 88.04(15) . .
C2 W1 P2 171.83(15) . .
C3 W1 P2 88.28(10) . .
C3 W1 P2 88.28(10) 4_565 .
P1 W1 P2 100.60(4) . .
C5 P1 C5 97.8(3) . 4_565
C5 P1 C7 97.31(16) . .
C5 P1 C7 97.31(16) 4_565 .
C5 P1 W1 122.66(12) . .
C5 P1 W1 122.66(12) 4_565 .
C7 P1 W1 113.66(17) . .
C11 P2 C17 102.54(14) . 4_565
C11 P2 C17 102.54(14) . .
C17 P2 C17 102.4(2) 4_565 .
C11 P2 W1 113.98(14) . .
C17 P2 W1 116.65(11) 4_565 .
C17 P2 W1 116.65(11) . .
C8 N1 C9 108.1(3) . .
C8 N1 C5 111.2(3) . .
C9 N1 C5 111.7(3) . .
C9 N3 C9 108.3(4) . 4_565
C9 N3 C7 111.1(2) . .
C9 N3 C7 111.1(2) 4_565 .
O1 C1 W1 176.4(5) . .
O2 C2 W1 174.5(5) . .
O3 C3 W1 174.2(3) . .
N1 C5 P1 112.6(2) . .
N1 C5 H5A 109.4 . .
P1 C5 H5A 109.1 . .
N1 C5 H5B 109.0 . .
P1 C5 H5B 109.0 . .
H5A C5 H5B 107.8 . .
N3 C7 P1 113.3(3) . .
N3 C7 H7A 108.8 . .
P1 C7 H7A 109.0 . .
N1 C8 N1 113.8(4) . 4_565
N1 C8 H8A 108.5 . .
N1 C8 H8A 108.5 4_565 .
N1 C8 H8B 109.1 . .
N1 C8 H8B 109.1 4_565 .
H8A C8 H8B 107.6 . .
N3 C9 N1 114.1(3) . .
N3 C9 H9A 108.3 . .
N1 C9 H9A 108.4 . .
N3 C9 H9B 109.0 . .
N1 C9 H9B 109.3 . .
H9A C9 H9B 107.6 . .
C12 C11 C12 118.1(5) 4_565 .
C12 C11 P2 120.7(2) 4_565 .
C12 C11 P2 120.7(2) . .
C13 C12 C11 121.0(4) . .
C13 C12 H12A 119.8 . .
C11 C12 H12A 119.2 . .
C14 C13 C12 120.4(4) . .
C14 C13 H13A 120.3 . .
C12 C13 H13A 119.4 . .
C13 C14 C13 119.0(5) . 4_565
C13 C14 H14A 120.5 . .
C13 C14 H14A 120.5 4_565 .
C22 C17 C18 118.6(3) . .
C22 C17 P2 120.2(3) . .
C18 C17 P2 121.1(3) . .
C19 C18 C17 120.7(3) . .
C19 C18 H18A 119.6 . .
C17 C18 H18A 119.7 . .
C20 C19 C18 120.2(3) . .
C20 C19 H19A 119.8 . .
C18 C19 H19A 120.0 . .
C21 C20 C19 119.6(3) . .
C21 C20 H20A 120.0 . .
C19 C20 H20A 120.4 . .
C20 C21 C22 120.4(3) . .
C20 C21 H21A 119.7 . .
C22 C21 H21A 119.8 . .
C17 C22 C21 120.4(3) . .
C17 C22 H22A 120.0 . .
C21 C22 H22A 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C1 1.995(5) .
W1 C2 2.009(5) .
W1 C3 2.026(4) .
W1 C3 2.026(4) 4_565
W1 P1 2.5043(13) .
W1 P2 2.5151(13) .
P1 C5 1.844(4) .
P1 C5 1.844(4) 4_565
P1 C7 1.854(5) .
P2 C11 1.823(5) .
P2 C17 1.847(3) 4_565
P2 C17 1.847(3) .
O1 C1 1.157(6) .
O2 C2 1.143(6) .
O3 C3 1.149(5) .
N1 C8 1.472(4) .
N1 C9 1.477(5) .
N1 C5 1.479(4) .
N3 C9 1.462(5) .
N3 C9 1.462(5) 4_565
N3 C7 1.475(6) .
C5 H5A 0.9882 .
C5 H5B 0.9888 .
C7 H7A 0.9881 .
C8 N1 1.472(4) 4_565
C8 H8A 0.9892 .
C8 H8B 0.9887 .
C9 H9A 0.9885 .
C9 H9B 0.9887 .
C11 C12 1.395(4) 4_565
C11 C12 1.395(4) .
C12 C13 1.394(5) .
C12 H12A 0.9487 .
C13 C14 1.392(5) .
C13 H13A 0.9489 .
C14 C13 1.392(5) 4_565
C14 H14A 0.9474 .
C17 C22 1.394(5) .
C17 C18 1.401(5) .
C18 C19 1.392(5) .
C18 H18A 0.9490 .
C19 C20 1.392(5) .
C19 H19A 0.9485 .
C20 C21 1.381(5) .
C20 H20A 0.9483 .
C21 C22 1.404(5) .
C21 H21A 0.9482 .
C22 H22A 0.9484 .
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 W1 P1 C5 -116.48(16) . .
C2 W1 P1 C5 -116.48(16) . .
C3 W1 P1 C5 150.54(19) . .
C3 W1 P1 C5 -23.50(19) 4_565 .
P2 W1 P1 C5 63.52(16) . .
C1 W1 P1 C5 116.48(16) . 4_565
C2 W1 P1 C5 116.48(16) . 4_565
C3 W1 P1 C5 23.50(19) . 4_565
C3 W1 P1 C5 -150.54(19) 4_565 4_565
P2 W1 P1 C5 -63.52(16) . 4_565
C1 W1 P1 C7 0.0 . .
C2 W1 P1 C7 0.0 . .
C3 W1 P1 C7 -92.98(10) . .
C3 W1 P1 C7 92.98(10) 4_565 .
P2 W1 P1 C7 180.0 . .
C1 W1 P2 C11 180.0 . .
C2 W1 P2 C11 180.000(1) . .
C3 W1 P2 C11 -83.09(10) . .
C3 W1 P2 C11 83.08(10) 4_565 .
P1 W1 P2 C11 0.0 . .
C1 W1 P2 C17 60.71(12) . 4_565
C2 W1 P2 C17 60.71(12) . 4_565
C3 W1 P2 C17 157.63(16) . 4_565
C3 W1 P2 C17 -36.20(16) 4_565 4_565
P1 W1 P2 C17 -119.29(12) . 4_565
C1 W1 P2 C17 -60.71(12) . .
C2 W1 P2 C17 -60.71(12) . .
C3 W1 P2 C17 36.20(16) . .
C3 W1 P2 C17 -157.63(16) 4_565 .
P1 W1 P2 C17 119.29(12) . .
C2 W1 C1 O1 0.00(2) . .
C3 W1 C1 O1 91.97(10) . .
C3 W1 C1 O1 -91.97(10) 4_565 .
P1 W1 C1 O1 0.00(2) . .
P2 W1 C1 O1 180.00(2) . .
C1 W1 C2 O2 0.000(15) . .
C3 W1 C2 O2 -96.60(10) . .
C3 W1 C2 O2 96.60(10) 4_565 .
P1 W1 C2 O2 180.000(15) . .
P2 W1 C2 O2 0.000(13) . .
C1 W1 C3 O3 160(3) . .
C2 W1 C3 O3 -116(3) . .
C3 W1 C3 O3 -4(4) 4_565 .
P1 W1 C3 O3 -28(3) . .
P2 W1 C3 O3 73(3) . .
C8 N1 C5 P1 60.6(4) . .
C9 N1 C5 P1 -60.3(4) . .
C5 P1 C5 N1 -49.4(4) 4_565 .
C7 P1 C5 N1 49.1(3) . .
W1 P1 C5 N1 173.3(2) . .
C9 N3 C7 P1 60.3(3) . .
C9 N3 C7 P1 -60.3(3) 4_565 .
C5 P1 C7 N3 -49.44(13) . .
C5 P1 C7 N3 49.44(13) 4_565 .
W1 P1 C7 N3 180.0 . .
C9 N1 C8 N1 55.8(5) . 4_565
C5 N1 C8 N1 -67.2(5) . 4_565
C9 N3 C9 N1 56.0(5) 4_565 .
C7 N3 C9 N1 -66.3(4) . .
C8 N1 C9 N3 -55.9(4) . .
C5 N1 C9 N3 66.8(4) . .
C17 P2 C11 C12 -146.7(3) 4_565 4_565
C17 P2 C11 C12 -40.7(4) . 4_565
W1 P2 C11 C12 86.3(3) . 4_565
C17 P2 C11 C12 40.8(4) 4_565 .
C17 P2 C11 C12 146.7(3) . .
W1 P2 C11 C12 -86.3(3) . .
C12 C11 C12 C13 1.0(6) 4_565 .
P2 C11 C12 C13 173.7(3) . .
C11 C12 C13 C14 -1.0(6) . .
C12 C13 C14 C13 1.0(7) . 4_565
C11 P2 C17 C22 139.7(3) . .
C17 P2 C17 C22 -114.2(2) 4_565 .
W1 P2 C17 C22 14.4(3) . .
C11 P2 C17 C18 -40.3(3) . .
C17 P2 C17 C18 65.8(3) 4_565 .
W1 P2 C17 C18 -165.6(2) . .
C22 C17 C18 C19 0.4(5) . .
P2 C17 C18 C19 -179.7(3) . .
C17 C18 C19 C20 -0.8(5) . .
C18 C19 C20 C21 0.3(5) . .
C19 C20 C21 C22 0.6(5) . .
C18 C17 C22 C21 0.6(5) . .
P2 C17 C22 C21 -179.4(3) . .
C20 C21 C22 C17 -1.0(5) . .
