#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:45:29 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178722 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/33/4083314.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_4083314
loop_
_publ_author_name
'Wang, Jinjin'
'Liu, Rui'
'Ruan, Wenqing'
'Li, Yan'
'Mondal, Kartik Chandra'
'Roesky, Herbert W.'
'Zhu, Hongping'
_publ_section_title
;
 N--P Bond Cleavage Induced Ring Formation of Cyclosilazanes from
 Reactions of Aryl(phosphanyl)aminotrichlorosilanes with Lithium Alkynyls
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2696
_journal_paper_doi               10.1021/om401095n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C48 H70 N2 Si2'
_chemical_formula_weight         731.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.79(3)
_cell_angle_beta                 92.59(3)
_cell_angle_gamma                114.44(3)
_cell_formula_units_Z            1
_cell_length_a                   10.662(2)
_cell_length_b                   11.188(2)
_cell_length_c                   11.882(2)
_cell_measurement_reflns_used    4598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.04
_cell_measurement_theta_min      6.20
_cell_volume                     1129.7(7)
_computing_cell_refinement       'rapid auto (rigaku 2004)'
_computing_data_collection       'rapid auto (rigaku 2004)'
_computing_data_reduction        'rapid auto (rigaku 2004)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'rigaku raxis rapid IP area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1047
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9044
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.9803
_exptl_absorpt_correction_type   'empirical absorption correction'
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment
'refined in a riding mode to the carrier atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3942
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                1700
_reflns_number_total             3942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401095n_si_002.cif
_cod_data_source_block           compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083311--4083318.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1129.7(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083314
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.92121(9) 0.06006(12) 0.49143(12) 0.0430(4) Uani 1 1 d . . .
N1 N 0.9115(3) -0.1106(3) 0.4451(3) 0.0372(8) Uani 1 1 d . . .
C1 C 0.8877(3) 0.1058(4) 0.3706(4) 0.0481(12) Uani 1 1 d . A .
C2 C 0.8550(4) 0.1459(5) 0.2963(5) 0.0678(15) Uani 1 1 d . . .
C3 C 0.8136(17) 0.1790(19) 0.1933(16) 0.079(4) Uani 0.644(18) 1 d PDU A 2
C4 C 0.8665(13) 0.3390(18) 0.2468(19) 0.104(4) Uani 0.644(18) 1 d PDU A 2
H4A H 0.8240 0.3735 0.3171 0.156 Uiso 0.644(18) 1 calc PR A 2
H4B H 0.8405 0.3601 0.1797 0.156 Uiso 0.644(18) 1 calc PR A 2
H4C H 0.9707 0.3914 0.2797 0.156 Uiso 0.644(18) 1 calc PR A 2
C5 C 0.8669(13) 0.113(2) 0.0713(15) 0.098(4) Uani 0.644(18) 1 d PDU A 2
H5A H 0.8198 0.0032 0.0325 0.148 Uiso 0.644(18) 1 calc PR A 2
H5B H 0.9706 0.1530 0.0971 0.148 Uiso 0.644(18) 1 calc PR A 2
H5C H 0.8433 0.1406 0.0085 0.148 Uiso 0.644(18) 1 calc PR A 2
C6 C 0.6618(11) 0.113(2) 0.1513(16) 0.094(4) Uani 0.644(18) 1 d PDU A 2
H6A H 0.6250 0.1521 0.2246 0.141 Uiso 0.644(18) 1 calc PR A 2
H6B H 0.6194 0.0038 0.1145 0.141 Uiso 0.644(18) 1 calc PR A 2
H6C H 0.6371 0.1368 0.0860 0.141 Uiso 0.644(18) 1 calc PR A 2
C3A C 0.819(3) 0.224(3) 0.238(3) 0.079(6) Uani 0.356(18) 1 d PDU A 1
C4A C 0.870(2) 0.390(3) 0.330(3) 0.107(6) Uani 0.356(18) 1 d PDU A 1
H4AA H 0.8275 0.4004 0.4026 0.160 Uiso 0.356(18) 1 calc PR A 1
H4AB H 0.8404 0.4335 0.2838 0.160 Uiso 0.356(18) 1 calc PR A 1
H4AC H 0.9741 0.4433 0.3613 0.160 Uiso 0.356(18) 1 calc PR A 1
C5A C 0.900(2) 0.214(4) 0.132(3) 0.103(6) Uani 0.356(18) 1 d PDU A 1
H5AA H 0.8968 0.1153 0.0912 0.155 Uiso 0.356(18) 1 calc PR A 1
H5AB H 1.0002 0.2924 0.1704 0.155 Uiso 0.356(18) 1 calc PR A 1
H5AC H 0.8557 0.2264 0.0668 0.155 Uiso 0.356(18) 1 calc PR A 1
C6A C 0.666(3) 0.169(3) 0.195(3) 0.098(6) Uiso 0.356(18) 1 d PDU A 1
H6AA H 0.6313 0.2139 0.2681 0.147 Uiso 0.356(18) 1 calc PR A 1
H6AB H 0.6152 0.0596 0.1582 0.147 Uiso 0.356(18) 1 calc PR A 1
H6AC H 0.6482 0.1957 0.1295 0.147 Uiso 0.356(18) 1 calc PR A 1
C11 C 0.8167(3) 0.1168(4) 0.5966(4) 0.0406(10) Uani 1 1 d . . .
C12 C 0.7404(4) 0.1627(5) 0.6594(4) 0.0511(12) Uani 1 1 d . . .
C13 C 0.6487(4) 0.2232(5) 0.7346(4) 0.0516(12) Uani 1 1 d . . .
C14 C 0.6917(5) 0.3776(5) 0.7590(6) 0.0795(16) Uani 1 1 d . . .
H14A H 0.6336 0.4150 0.8097 0.119 Uiso 1 1 calc R . .
H14B H 0.6774 0.3775 0.6768 0.119 Uiso 1 1 calc R . .
H14C H 0.7928 0.4427 0.8064 0.119 Uiso 1 1 calc R . .
C15 C 0.5018(4) 0.1372(6) 0.6602(5) 0.0822(17) Uani 1 1 d . . .
H15A H 0.4459 0.1820 0.7074 0.123 Uiso 1 1 calc R . .
H15B H 0.4634 0.0340 0.6449 0.123 Uiso 1 1 calc R . .
H15C H 0.4961 0.1373 0.5776 0.123 Uiso 1 1 calc R . .
C16 C 0.6606(5) 0.2192(6) 0.8597(5) 0.0751(15) Uani 1 1 d . . .
H16A H 0.5943 0.2484 0.9036 0.113 Uiso 1 1 calc R . .
H16B H 0.7585 0.2890 0.9144 0.113 Uiso 1 1 calc R . .
H16C H 0.6367 0.1175 0.8424 0.113 Uiso 1 1 calc R . .
C21 C 0.8007(3) -0.2470(4) 0.3766(5) 0.0452(11) Uani 1 1 d . . .
C22 C 0.7736(4) -0.3153(5) 0.2457(5) 0.0541(12) Uani 1 1 d . . .
C23 C 0.6641(4) -0.4449(5) 0.1846(5) 0.0674(15) Uani 1 1 d . . .
H23A H 0.6388 -0.5001 0.0934 0.081 Uiso 1 1 calc R . .
C24 C 0.5853(4) -0.5013(5) 0.2531(7) 0.0752(17) Uani 1 1 d . . .
H24A H 0.5037 -0.5974 0.2074 0.090 Uiso 1 1 calc R . .
C25 C 0.6152(4) -0.4298(5) 0.3821(6) 0.0705(16) Uani 1 1 d . . .
H25A H 0.5550 -0.4766 0.4239 0.085 Uiso 1 1 calc R . .
C26 C 0.7218(3) -0.3014(5) 0.4488(5) 0.0528(13) Uani 1 1 d . . .
C221 C 0.8583(4) -0.2616(5) 0.1675(4) 0.0587(13) Uani 1 1 d . . .
H22A H 0.9369 -0.1588 0.2288 0.070 Uiso 1 1 calc R . .
C222 C 0.7741(5) -0.2426(6) 0.0732(5) 0.0826(17) Uani 1 1 d . . .
H22B H 0.7338 -0.1781 0.1206 0.124 Uiso 1 1 calc R . .
H22C H 0.6967 -0.3408 0.0091 0.124 Uiso 1 1 calc R . .
H22D H 0.8383 -0.1966 0.0299 0.124 Uiso 1 1 calc R . .
C223 C 0.9333(4) -0.3575(6) 0.1019(5) 0.0806(17) Uani 1 1 d . . .
H22E H 0.9943 -0.3548 0.1681 0.121 Uiso 1 1 calc R . .
H22F H 0.9917 -0.3163 0.0528 0.121 Uiso 1 1 calc R . .
H22G H 0.8606 -0.4613 0.0438 0.121 Uiso 1 1 calc R . .
C261 C 0.7469(4) -0.2325(5) 0.5900(5) 0.0596(14) Uani 1 1 d . . .
H26A H 0.8366 -0.1346 0.6260 0.072 Uiso 1 1 calc R . .
C262 C 0.7787(4) -0.3262(6) 0.6430(6) 0.0835(18) Uani 1 1 d . . .
H26B H 0.8588 -0.3403 0.6147 0.125 Uiso 1 1 calc R . .
H26C H 0.6939 -0.4241 0.6105 0.125 Uiso 1 1 calc R . .
H26D H 0.8033 -0.2730 0.7372 0.125 Uiso 1 1 calc R . .
C263 C 0.6286(4) -0.1939(5) 0.6407(5) 0.0694(15) Uani 1 1 d . . .
H26E H 0.6207 -0.1250 0.6138 0.104 Uiso 1 1 calc R . .
H26F H 0.6539 -0.1464 0.7348 0.104 Uiso 1 1 calc R . .
H26G H 0.5369 -0.2860 0.6053 0.104 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'
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
N1 Si1 N1 79.07(15) 2_756 .
N1 Si1 C1 118.64(15) 2_756 .
N1 Si1 C1 118.7(2) . .
N1 Si1 C11 119.06(18) 2_756 .
N1 Si1 C11 119.44(16) . .
C1 Si1 C11 102.23(19) . .
N1 Si1 Si1 40.18(11) 2_756 2_756
N1 Si1 Si1 38.89(9) . 2_756
C1 Si1 Si1 128.45(16) . 2_756
C11 Si1 Si1 129.32(14) . 2_756
C21 N1 Si1 129.4(3) . 2_756
C21 N1 Si1 129.7(2) . .
Si1 N1 Si1 100.93(15) 2_756 .
C2 C1 Si1 171.7(4) . .
C1 C2 C3A 165.6(12) . .
C1 C2 C3 173.6(9) . .
C3A C2 C3 20.8(13) . .
C4 C3 C6 105.5(13) . .
C4 C3 C2 109.7(10) . .
C6 C3 C2 110.6(10) . .
C4 C3 C5 112.3(11) . .
C6 C3 C5 107.2(11) . .
C2 C3 C5 111.4(12) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C2 C3A C6A 114(2) . .
C2 C3A C5A 103(2) . .
C6A C3A C5A 115(2) . .
C2 C3A C4A 115(2) . .
C6A C3A C4A 101(2) . .
C5A C3A C4A 108(2) . .
C12 C11 Si1 171.9(3) . .
C11 C12 C13 177.9(4) . .
C15 C13 C14 104.6(4) . .
C15 C13 C16 110.3(4) . .
C14 C13 C16 110.3(4) . .
C15 C13 C12 110.7(4) . .
C14 C13 C12 111.1(3) . .
C16 C13 C12 109.7(4) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N1 C21 C22 118.5(3) . .
N1 C21 C26 114.3(4) . .
C22 C21 C26 127.2(4) . .
C23 C22 C21 115.9(4) . .
C23 C22 C221 116.1(5) . .
C21 C22 C221 128.0(4) . .
C22 C23 C24 118.2(5) . .
C22 C23 H23A 120.9 . .
C24 C23 H23A 120.9 . .
C25 C24 C23 124.1(4) . .
C25 C24 H24A 118.0 . .
C23 C24 H24A 118.0 . .
C26 C25 C24 121.3(5) . .
C26 C25 H25A 119.4 . .
C24 C25 H25A 119.4 . .
C25 C26 C21 113.5(5) . .
C25 C26 C261 117.3(4) . .
C21 C26 C261 129.2(3) . .
C22 C221 C222 112.9(4) . .
C22 C221 C223 111.6(4) . .
C222 C221 C223 113.6(4) . .
C22 C221 H22A 106.0 . .
C222 C221 H22A 106.0 . .
C223 C221 H22A 106.0 . .
C221 C222 H22B 109.5 . .
C221 C222 H22C 109.5 . .
H22B C222 H22C 109.5 . .
C221 C222 H22D 109.5 . .
H22B C222 H22D 109.5 . .
H22C C222 H22D 109.5 . .
C221 C223 H22E 109.5 . .
C221 C223 H22F 109.5 . .
H22E C223 H22F 109.5 . .
C221 C223 H22G 109.5 . .
H22E C223 H22G 109.5 . .
H22F C223 H22G 109.5 . .
C26 C261 C262 111.6(4) . .
C26 C261 C263 114.3(4) . .
C262 C261 C263 112.4(3) . .
C26 C261 H26A 105.9 . .
C262 C261 H26A 105.9 . .
C263 C261 H26A 105.9 . .
C261 C262 H26B 109.5 . .
C261 C262 H26C 109.5 . .
H26B C262 H26C 109.5 . .
C261 C262 H26D 109.5 . .
H26B C262 H26D 109.5 . .
H26C C262 H26D 109.5 . .
C261 C263 H26E 109.5 . .
C261 C263 H26F 109.5 . .
H26E C263 H26F 109.5 . .
C261 C263 H26G 109.5 . .
H26E C263 H26G 109.5 . .
H26F C263 H26G 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N1 1.660(3) 2_756
Si1 N1 1.706(3) .
Si1 C1 1.781(4) .
Si1 C11 1.804(5) .
Si1 Si1 2.596(2) 2_756
N1 C21 1.330(4) .
N1 Si1 1.660(3) 2_756
C1 C2 1.239(5) .
C2 C3A 1.47(4) .
C2 C3 1.516(18) .
C3 C4 1.450(17) .
C3 C6 1.428(16) .
C3 C5 1.580(16) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C3A C6A 1.46(3) .
C3A C5A 1.56(3) .
C3A C4A 1.53(3) .
C4A H4AA 0.9800 .
C4A H4AB 0.9800 .
C4A H4AC 0.9800 .
C5A H5AA 0.9800 .
C5A H5AB 0.9800 .
C5A H5AC 0.9800 .
C6A H6AA 0.9800 .
C6A H6AB 0.9800 .
C6A H6AC 0.9800 .
C11 C12 1.249(6) .
C12 C13 1.527(6) .
C13 C15 1.441(5) .
C13 C14 1.481(6) .
C13 C16 1.507(6) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C21 C22 1.366(6) .
C21 C26 1.376(5) .
C22 C23 1.278(5) .
C22 C221 1.461(6) .
C23 C24 1.349(7) .
C23 H23A 0.9500 .
C24 C25 1.345(7) .
C24 H24A 0.9500 .
C25 C26 1.263(5) .
C25 H25A 0.9500 .
C26 C261 1.478(6) .
C221 C222 1.540(6) .
C221 C223 1.569(7) .
C221 H22A 1.0000 .
C222 H22B 0.9800 .
C222 H22C 0.9800 .
C222 H22D 0.9800 .
C223 H22E 0.9800 .
C223 H22F 0.9800 .
C223 H22G 0.9800 .
C261 C262 1.562(6) .
C261 C263 1.563(6) .
C261 H26A 1.0000 .
C262 H26B 0.9800 .
C262 H26C 0.9800 .
C262 H26D 0.9800 .
C263 H26E 0.9800 .
C263 H26F 0.9800 .
C263 H26G 0.9800 .
