#------------------------------------------------------------------------------
#$Date: 2017-10-14 21:27:35 +0200 (Sat 14 de Oct de 2017) $
#$Revision: 202017 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/00/7000095.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_7000095
loop_
_publ_author_name
'Schranz, Ingo'
'Lief, Graham R.'
'Carrow, Christopher J.'
'Haagenson, Dana C.'
'Grocholl, Luke'
'Stahl, Lothar'
'Staples, Richard J.'
'Boomishankar, Ramamoorthy'
'Steiner, Alexander'
_publ_section_title
;
 Reversal of polarization in amidophosphines: neutral- and
 anionic-kappaP coordination vs. anionic-kappaP,N coordination and the
 formation of nickelaazaphosphiranes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3307
_journal_page_last               3318
_journal_paper_doi               10.1039/b507040f
_journal_year                    2005
_chemical_formula_sum            'C26 H54 N6 P2 Si2'
_chemical_formula_weight         568.87
_chemical_name_systematic
;
?
;
_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                 109.808(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2122(13)
_cell_length_b                   33.045(5)
_cell_length_c                   12.3486(16)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      5.20
_cell_volume                     3536.7(9)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5826
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0965P)²+2.4714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                3849
_reflns_number_total             4593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b507040f.txt
_cod_data_source_block           9a
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3536.7(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7000095
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
P1 P 0.11862(12) 0.44715(3) 0.76602(8) 0.0700(3) Uani 1 1 d . . .
P2 P 0.50123(11) 0.31539(3) 1.06885(8) 0.0657(3) Uani 1 1 d . . .
Si1 Si 0.17411(13) 0.42669(3) 0.58424(8) 0.0695(3) Uani 1 1 d . . .
Si2 Si 0.62672(13) 0.28173(3) 0.93641(10) 0.0736(3) Uani 1 1 d . . .
N1 N 0.1890(4) 0.41011(10) 0.8662(2) 0.0868(10) Uani 1 1 d . . .
H1 H 0.2072 0.3872 0.8402 0.104 Uiso 1 1 calc R . .
N2 N 0.4074(4) 0.35838(9) 1.0097(2) 0.0775(9) Uani 1 1 d . . .
H2N H 0.4084 0.3643 0.9422 0.093 Uiso 1 1 calc R . .
N3 N 0.0351(4) 0.41849(9) 0.6454(2) 0.0722(8) Uani 1 1 d . . .
N4 N 0.2582(4) 0.45523(9) 0.7054(2) 0.0706(8) Uani 1 1 d . . .
N5 N 0.4527(4) 0.28118(9) 0.9579(3) 0.0743(8) Uani 1 1 d . . .
N6 N 0.6695(3) 0.31892(9) 1.0399(3) 0.0693(8) Uani 1 1 d . . .
C1 C 0.2211(4) 0.41207(10) 0.9857(3) 0.0643(9) Uani 1 1 d . . .
C2 C 0.1456(5) 0.43926(11) 1.0335(3) 0.0764(10) Uani 1 1 d . . .
H2 H 0.0748 0.4573 0.9860 0.092 Uiso 1 1 calc R . .
C3 C 0.1736(5) 0.44008(12) 1.1501(3) 0.0819(11) Uani 1 1 d . . .
H3 H 0.1229 0.4587 1.1811 0.098 Uiso 1 1 calc R . .
C4 C 0.2760(5) 0.41346(13) 1.2201(3) 0.0832(11) Uani 1 1 d . . .
H4 H 0.2931 0.4134 1.2987 0.100 Uiso 1 1 calc R . .
C5 C 0.3538(4) 0.38675(12) 1.1748(3) 0.0762(10) Uani 1 1 d . . .
H5 H 0.4251 0.3691 1.2236 0.091 Uiso 1 1 calc R . .
C6 C 0.3283(4) 0.38551(10) 1.0573(3) 0.0603(8) Uani 1 1 d . . .
C7 C 0.2797(7) 0.38077(15) 0.5662(5) 0.1200(18) Uani 1 1 d . . .
H7A H 0.3095 0.3652 0.6359 0.180 Uiso 1 1 calc R . .
H7B H 0.3702 0.3886 0.5494 0.180 Uiso 1 1 calc R . .
H7C H 0.2141 0.3648 0.5039 0.180 Uiso 1 1 calc R . .
C8 C 0.1106(6) 0.45416(13) 0.4451(3) 0.0922(13) Uani 1 1 d . . .
H8A H 0.0415 0.4374 0.3868 0.138 Uiso 1 1 calc R . .
H8B H 0.1989 0.4607 0.4239 0.138 Uiso 1 1 calc R . .
H8C H 0.0587 0.4786 0.4526 0.138 Uiso 1 1 calc R . .
C9 C 0.6254(6) 0.29614(17) 0.7917(4) 0.1087(15) Uani 1 1 d . . .
H9A H 0.5872 0.2740 0.7396 0.163 Uiso 1 1 calc R . .
H9B H 0.7284 0.3027 0.7952 0.163 Uiso 1 1 calc R . .
H9C H 0.5599 0.3193 0.7652 0.163 Uiso 1 1 calc R . .
C10 C 0.7428(7) 0.23449(15) 0.9792(5) 0.1273(19) Uani 1 1 d . . .
H10A H 0.7412 0.2256 1.0528 0.191 Uiso 1 1 calc R . .
H10B H 0.8473 0.2397 0.9840 0.191 Uiso 1 1 calc R . .
H10C H 0.6996 0.2138 0.9228 0.191 Uiso 1 1 calc R . .
C11 C -0.1178(5) 0.40010(14) 0.6099(4) 0.0949(13) Uani 1 1 d . . .
C12 C -0.1563(12) 0.3833(5) 0.4926(8) 0.313(9) Uani 1 1 d . . .
H12A H -0.2546 0.3700 0.4711 0.469 Uiso 1 1 calc R . .
H12B H -0.0785 0.3642 0.4911 0.469 Uiso 1 1 calc R . .
H12C H -0.1607 0.4049 0.4394 0.469 Uiso 1 1 calc R . .
C13 C -0.2286(9) 0.4295(3) 0.6051(18) 0.427(14) Uani 1 1 d . . .
H13A H -0.2048 0.4539 0.5723 0.641 Uiso 1 1 calc R . .
H13B H -0.2289 0.4349 0.6814 0.641 Uiso 1 1 calc R . .
H13C H -0.3285 0.4199 0.5582 0.641 Uiso 1 1 calc R . .
C14 C -0.1265(13) 0.3681(4) 0.6812(9) 0.335(10) Uani 1 1 d . . .
H14A H -0.1381 0.3786 0.7503 0.502 Uiso 1 1 calc R . .
H14B H -0.0338 0.3523 0.7005 0.502 Uiso 1 1 calc R . .
H14C H -0.2137 0.3514 0.6418 0.502 Uiso 1 1 calc R . .
C15 C 0.3995(5) 0.47873(13) 0.7548(4) 0.0905(12) Uani 1 1 d . . .
C16 C 0.5202(6) 0.4533(2) 0.8450(6) 0.150(3) Uani 1 1 d . . .
H16A H 0.4847 0.4477 0.9081 0.225 Uiso 1 1 calc R . .
H16B H 0.6157 0.4680 0.8724 0.225 Uiso 1 1 calc R . .
H16C H 0.5359 0.4283 0.8109 0.225 Uiso 1 1 calc R . .
C17 C 0.3664(8) 0.51733(17) 0.8091(6) 0.142(2) Uani 1 1 d . . .
H17A H 0.2927 0.5334 0.7514 0.213 Uiso 1 1 calc R . .
H17B H 0.4602 0.5324 0.8416 0.213 Uiso 1 1 calc R . .
H17C H 0.3253 0.5106 0.8687 0.213 Uiso 1 1 calc R . .
C18 C 0.4618(7) 0.4893(2) 0.6600(5) 0.133(2) Uani 1 1 d . . .
H18A H 0.4717 0.4651 0.6200 0.199 Uiso 1 1 calc R . .
H18B H 0.5611 0.5019 0.6926 0.199 Uiso 1 1 calc R . .
H18C H 0.3922 0.5077 0.6071 0.199 Uiso 1 1 calc R . .
C19 C 0.3078(5) 0.25860(13) 0.9105(4) 0.0831(11) Uani 1 1 d . . .
C20 C 0.1954(8) 0.2825(2) 0.8189(7) 0.186(4) Uani 1 1 d . . .
H20A H 0.1443 0.3014 0.8528 0.278 Uiso 1 1 calc R . .
H20B H 0.1204 0.2646 0.7683 0.278 Uiso 1 1 calc R . .
H20C H 0.2482 0.2969 0.7759 0.278 Uiso 1 1 calc R . .
C21 C 0.3413(8) 0.2180(2) 0.8615(8) 0.182(3) Uani 1 1 d . . .
H21A H 0.3831 0.2232 0.8015 0.272 Uiso 1 1 calc R . .
H21B H 0.2473 0.2029 0.8309 0.272 Uiso 1 1 calc R . .
H21C H 0.4144 0.2028 0.9218 0.272 Uiso 1 1 calc R . .
C22 C 0.2433(7) 0.2473(2) 1.0027(6) 0.153(3) Uani 1 1 d . . .
H22A H 0.3186 0.2320 1.0613 0.230 Uiso 1 1 calc R . .
H22B H 0.1520 0.2312 0.9699 0.230 Uiso 1 1 calc R . .
H22C H 0.2179 0.2714 1.0359 0.230 Uiso 1 1 calc R . .
C23 C 0.8105(5) 0.33982(13) 1.1103(4) 0.0869(12) Uani 1 1 d . . .
C24 C 0.7761(7) 0.38339(17) 1.1323(7) 0.156(3) Uani 1 1 d . . .
H24A H 0.7412 0.3979 1.0606 0.233 Uiso 1 1 calc R . .
H24B H 0.8681 0.3959 1.1831 0.233 Uiso 1 1 calc R . .
H24C H 0.6973 0.3840 1.1669 0.233 Uiso 1 1 calc R . .
C26 C 0.9287(7) 0.3371(2) 1.0526(6) 0.169(3) Uani 1 1 d . . .
H26A H 0.9500 0.3092 1.0425 0.254 Uiso 1 1 calc R . .
H26B H 1.0217 0.3503 1.0993 0.254 Uiso 1 1 calc R . .
H26C H 0.8903 0.3502 0.9788 0.254 Uiso 1 1 calc R . .
C25 C 0.8746(8) 0.3192(2) 1.2276(6) 0.174(3) Uani 1 1 d . . .
H25A H 0.7982 0.3197 1.2646 0.260 Uiso 1 1 calc R . .
H25B H 0.9652 0.3333 1.2745 0.260 Uiso 1 1 calc R . .
H25C H 0.9007 0.2917 1.2176 0.260 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
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
C C 0.0033 0.0016 '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
N1 P1 N3 100.49(16) . . ?
N1 P1 N4 105.76(17) . . ?
N3 P1 N4 83.62(15) . . ?
N1 P1 Si1 107.89(11) . . ?
N3 P1 Si1 41.79(11) . . ?
N4 P1 Si1 41.83(10) . . ?
N2 P2 N6 102.65(15) . . ?
N2 P2 N5 104.57(16) . . ?
N6 P2 N5 83.55(15) . . ?
N2 P2 Si2 111.37(11) . . ?
N6 P2 Si2 41.99(10) . . ?
N5 P2 Si2 41.73(11) . . ?
N3 Si1 N4 83.47(15) . . ?
N3 Si1 C8 115.97(19) . . ?
N4 Si1 C8 116.54(18) . . ?
N3 Si1 C7 115.1(2) . . ?
N4 Si1 C7 117.0(2) . . ?
C8 Si1 C7 107.6(2) . . ?
N3 Si1 P1 41.70(10) . . ?
N4 Si1 P1 41.77(11) . . ?
C8 Si1 P1 126.18(14) . . ?
C7 Si1 P1 126.20(18) . . ?
N5 Si2 N6 83.31(14) . . ?
N5 Si2 C9 117.0(2) . . ?
N6 Si2 C9 117.4(2) . . ?
N5 Si2 C10 115.1(2) . . ?
N6 Si2 C10 115.0(2) . . ?
C9 Si2 C10 107.8(3) . . ?
N5 Si2 P2 41.82(10) . . ?
N6 Si2 P2 41.66(10) . . ?
C9 Si2 P2 130.64(18) . . ?
C10 Si2 P2 121.57(19) . . ?
C1 N1 P1 128.5(2) . . ?
C6 N2 P2 128.0(2) . . ?
C11 N3 P1 126.5(3) . . ?
C11 N3 Si1 136.3(3) . . ?
P1 N3 Si1 96.51(16) . . ?
C15 N4 P1 126.5(3) . . ?
C15 N4 Si1 137.1(3) . . ?
P1 N4 Si1 96.40(16) . . ?
C19 N5 Si2 135.8(3) . . ?
C19 N5 P2 127.6(3) . . ?
Si2 N5 P2 96.45(15) . . ?
C23 N6 P2 126.3(3) . . ?
C23 N6 Si2 135.3(3) . . ?
P2 N6 Si2 96.35(15) . . ?
C2 C1 C6 119.2(3) . . ?
C2 C1 N1 121.4(3) . . ?
C6 C1 N1 119.4(3) . . ?
C3 C2 C1 121.1(4) . . ?
C4 C3 C2 119.7(4) . . ?
C3 C4 C5 120.2(4) . . ?
C4 C5 C6 121.2(4) . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 N2 121.8(3) . . ?
C1 C6 N2 119.6(3) . . ?
C14 C11 C13 110.9(10) . . ?
C14 C11 N3 112.5(5) . . ?
C13 C11 N3 110.0(5) . . ?
C14 C11 C12 106.7(8) . . ?
C13 C11 C12 106.9(9) . . ?
N3 C11 C12 109.7(5) . . ?
N4 C15 C18 108.6(4) . . ?
N4 C15 C17 110.3(4) . . ?
C18 C15 C17 109.5(5) . . ?
N4 C15 C16 109.7(4) . . ?
C18 C15 C16 108.5(5) . . ?
C17 C15 C16 110.2(5) . . ?
N5 C19 C20 109.9(4) . . ?
N5 C19 C22 111.4(4) . . ?
C20 C19 C22 111.1(5) . . ?
N5 C19 C21 108.8(4) . . ?
C20 C19 C21 110.2(6) . . ?
C22 C19 C21 105.3(5) . . ?
N6 C23 C26 109.4(4) . . ?
N6 C23 C24 110.8(4) . . ?
C26 C23 C24 111.8(5) . . ?
N6 C23 C25 109.4(4) . . ?
C26 C23 C25 108.5(5) . . ?
C24 C23 C25 106.9(5) . . ?
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
P1 N1 1.704(3) . ?
P1 N3 1.712(3) . ?
P1 N4 1.714(3) . ?
P1 Si1 2.5564(13) . ?
P2 N2 1.694(3) . ?
P2 N6 1.709(3) . ?
P2 N5 1.715(3) . ?
P2 Si2 2.5553(14) . ?
Si1 N3 1.715(3) . ?
Si1 N4 1.716(3) . ?
Si1 C8 1.854(4) . ?
Si1 C7 1.856(4) . ?
Si2 N5 1.712(3) . ?
Si2 N6 1.720(3) . ?
Si2 C9 1.845(4) . ?
Si2 C10 1.865(5) . ?
N1 C1 1.405(4) . ?
N2 C6 1.404(4) . ?
N3 C11 1.459(5) . ?
N4 C15 1.460(5) . ?
N5 C19 1.467(5) . ?
N6 C23 1.468(5) . ?
C1 C2 1.385(5) . ?
C1 C6 1.391(5) . ?
C2 C3 1.373(5) . ?
C3 C4 1.363(6) . ?
C4 C5 1.370(5) . ?
C5 C6 1.390(5) . ?
C11 C14 1.395(8) . ?
C11 C13 1.395(9) . ?
C11 C12 1.478(10) . ?
C15 C18 1.510(7) . ?
C15 C17 1.519(7) . ?
C15 C16 1.530(7) . ?
C19 C20 1.477(7) . ?
C19 C22 1.499(7) . ?
C19 C21 1.545(7) . ?
C23 C26 1.492(7) . ?
C23 C24 1.518(7) . ?
C23 C25 1.526(7) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21144935
