#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:56:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179270 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/90/4319019.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_4319019
loop_
_publ_author_name
'Ingo Schranz'
'Graham R. Lief'
'Steven J. Midstokke'
'Lothar Stahl'
_publ_contact_author_address
;  Department of Chemistry
    University of North Dakota
    Grand Forks, ND 585620
    USA
;
_publ_contact_author_email       lstahl@chem.und.edu
_publ_contact_author_fax         '(701) 777-2331'
_publ_contact_author_name        'Lothar Stahl'
_publ_contact_author_phone       '(701) 777-2242'
_publ_section_title
;
 Inorganic Heterocyclic Bis(phosphines): Syntheses and Structures of a
 1,2-Bis(diazasilaphosphetidino)ethane and Its Nickel, Molybdenum, and
 Rhodium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6919
_journal_page_last               6927
_journal_paper_doi               10.1021/ic020524v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C22 H52 N4 P2 Si2'
_chemical_formula_weight         490.80
_chemical_name_systematic        PhetPhos
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.147(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5368(16)
_cell_length_b                   10.4604(17)
_cell_length_c                   12.6864(14)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      12.77
_cell_measurement_theta_min      4.31
_cell_volume                     1518.1(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      292(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3400
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         1.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0690P)²+0.4708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                2310
_reflns_number_total             2656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020524v_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319019
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.20261(13) 0.34608(15) 0.15579(15) 0.0468(4) Uani 1 1 d . . .
N2 N 0.21498(13) 0.55914(15) 0.21265(14) 0.0448(4) Uani 1 1 d . . .
P1 P 0.11126(4) 0.44287(5) 0.19306(5) 0.04586(19) Uani 1 1 d . . .
Si1 Si 0.31335(4) 0.45614(5) 0.19591(5) 0.0466(2) Uani 1 1 d . . .
C1 C 0.44314(19) 0.4183(3) 0.3327(2) 0.0705(7) Uani 1 1 d . . .
H1A H 0.4175 0.3988 0.3926 0.106 Uiso 1 1 calc R . .
H1B H 0.4947 0.4907 0.3553 0.106 Uiso 1 1 calc R . .
H1C H 0.4838 0.3459 0.3204 0.106 Uiso 1 1 calc R . .
C2 C 0.3656(2) 0.5011(3) 0.0824(2) 0.0735(7) Uani 1 1 d . . .
H2A H 0.4090 0.4313 0.0702 0.110 Uiso 1 1 calc R . .
H2B H 0.4151 0.5750 0.1072 0.110 Uiso 1 1 calc R . .
H2C H 0.2997 0.5200 0.0116 0.110 Uiso 1 1 calc R . .
C3 C -0.01170(16) 0.4816(2) 0.05217(18) 0.0497(5) Uani 1 1 d . . .
H3A H -0.0632 0.4079 0.0302 0.060 Uiso 1 1 calc R . .
H3B H -0.0554 0.5512 0.0662 0.060 Uiso 1 1 calc R . .
C10 C 0.20312(19) 0.20532(19) 0.16038(19) 0.0562(5) Uani 1 1 d . . .
C11 C 0.2334(3) 0.1581(3) 0.2842(3) 0.0907(9) Uani 1 1 d . . .
H11A H 0.3104 0.1867 0.3340 0.136 Uiso 1 1 calc R . .
H11B H 0.2310 0.0664 0.2847 0.136 Uiso 1 1 calc R . .
H11C H 0.1777 0.1917 0.3110 0.136 Uiso 1 1 calc R . .
C12 C 0.2931(3) 0.1574(3) 0.1181(3) 0.0971(10) Uani 1 1 d . . .
H12A H 0.2697 0.1811 0.0386 0.146 Uiso 1 1 calc R . .
H12B H 0.2987 0.0660 0.1250 0.146 Uiso 1 1 calc R . .
H12C H 0.3678 0.1947 0.1638 0.146 Uiso 1 1 calc R . .
C13 C 0.0862(3) 0.1548(3) 0.0802(3) 0.1026(12) Uani 1 1 d . . .
H13A H 0.0268 0.1893 0.1014 0.154 Uiso 1 1 calc R . .
H13B H 0.0862 0.0633 0.0853 0.154 Uiso 1 1 calc R . .
H13C H 0.0708 0.1796 0.0024 0.154 Uiso 1 1 calc R . .
C20 C 0.22929(18) 0.67592(19) 0.28291(18) 0.0513(5) Uani 1 1 d . . .
C21 C 0.1223(2) 0.7587(3) 0.2273(3) 0.0851(9) Uani 1 1 d . . .
H21A H 0.1142 0.7837 0.1516 0.128 Uiso 1 1 calc R . .
H21B H 0.1302 0.8336 0.2737 0.128 Uiso 1 1 calc R . .
H21C H 0.0543 0.7116 0.2213 0.128 Uiso 1 1 calc R . .
C22 C 0.3325(3) 0.7499(3) 0.2829(3) 0.0895(9) Uani 1 1 d . . .
H22A H 0.4021 0.6992 0.3181 0.134 Uiso 1 1 calc R . .
H22B H 0.3412 0.8277 0.3257 0.134 Uiso 1 1 calc R . .
H22C H 0.3200 0.7697 0.2048 0.134 Uiso 1 1 calc R . .
C23 C 0.2481(3) 0.6440(3) 0.4081(2) 0.0805(8) Uani 1 1 d . . .
H23A H 0.1843 0.5926 0.4072 0.121 Uiso 1 1 calc R . .
H23B H 0.2517 0.7218 0.4496 0.121 Uiso 1 1 calc R . .
H23C H 0.3200 0.5977 0.4454 0.121 Uiso 1 1 calc 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'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
C10 N1 Si1 132.07(14) . . ?
C10 N1 P1 124.46(15) . . ?
Si1 N1 P1 94.13(8) . . ?
C20 N2 Si1 132.63(13) . . ?
C20 N2 P1 124.63(13) . . ?
Si1 N2 P1 94.43(8) . . ?
N2 P1 N1 84.71(8) . . ?
N2 P1 C3 105.31(9) . . ?
N1 P1 C3 104.17(9) . . ?
N2 P1 Si1 42.67(5) . . ?
N1 P1 Si1 42.63(6) . . ?
C3 P1 Si1 115.67(7) . . ?
N1 Si1 N2 85.56(8) . . ?
N1 Si1 C2 115.91(11) . . ?
N2 Si1 C2 115.71(11) . . ?
N1 Si1 C1 115.12(11) . . ?
N2 Si1 C1 114.48(10) . . ?
C2 Si1 C1 108.75(12) . . ?
N1 Si1 P1 43.25(6) . . ?
N2 Si1 P1 42.90(5) . . ?
C2 Si1 P1 132.00(9) . . ?
C1 Si1 P1 119.24(9) . . ?
C3 C3 P1 120.78(17) 3_565 . ?
N1 C10 C13 109.77(19) . . ?
N1 C10 C12 107.9(2) . . ?
C13 C10 C12 107.8(2) . . ?
N1 C10 C11 110.88(19) . . ?
C13 C10 C11 110.2(3) . . ?
C12 C10 C11 110.3(2) . . ?
N2 C20 C22 108.42(18) . . ?
N2 C20 C21 109.10(18) . . ?
C22 C20 C21 107.7(2) . . ?
N2 C20 C23 111.78(18) . . ?
C22 C20 C23 109.9(2) . . ?
C21 C20 C23 109.8(2) . . ?
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
N1 C10 1.473(3) . ?
N1 Si1 1.7129(17) . ?
N1 P1 1.7329(17) . ?
N2 C20 1.479(3) . ?
N2 Si1 1.7149(16) . ?
N2 P1 1.7225(16) . ?
P1 C3 1.866(2) . ?
P1 Si1 2.5227(8) . ?
Si1 C2 1.870(2) . ?
Si1 C1 1.873(2) . ?
C3 C3 1.518(4) 3_565 ?
C10 C13 1.497(3) . ?
C10 C12 1.519(4) . ?
C10 C11 1.538(4) . ?
C20 C22 1.508(3) . ?
C20 C21 1.508(3) . ?
C20 C23 1.544(3) . ?
