#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:47:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178534 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/39/4063971.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_4063971
loop_
_publ_author_name
'Sarish, Sankaranarayana Pillai'
'Jana, Anukul'
'Roesky, Herbert W.'
'Samuel, Prinson P.'
'Andrade, Carlos E. Abad'
'Dittrich, Birger'
'Schulzke, Carola'
_publ_contact_author
;
Dittrich, Birger, Institute for Inorganic Chemistry,
Georg-August-University Goettingen, Tammannstr. 4,
D-37077 Goettingen, Germany.
;
_publ_section_title
;
 Synthesis of a Lewis Base Stabilized Dimer of N-Substituted Hydrosila
 Hydrazone and a Silaaziridine
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              912
_journal_paper_doi               10.1021/om101066w
_journal_volume                  30
_journal_year                    2011
_chemical_compound_source        ' Synthesis '
_chemical_formula_moiety         'C56 H68 N8 Si2, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H84 N8 O2 Si2'
_chemical_formula_weight         1053.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 113.1287(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7543(3)
_cell_length_b                   18.2098(4)
_cell_length_c                   13.9106(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0
_cell_measurement_theta_min      3.75
_cell_volume                     2971.11(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2008)'
_computing_data_collection       'Apex2 (Bruker AXS, 2008)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_UB_11      2.8607631e-02
_diffrn_orient_matrix_UB_12      3.5793826e-02
_diffrn_orient_matrix_UB_13      5.9195384e-02
_diffrn_orient_matrix_UB_21      -7.8925155e-02
_diffrn_orient_matrix_UB_22      1.9871533e-02
_diffrn_orient_matrix_UB_23      -2.0521937e-02
_diffrn_orient_matrix_UB_31      -1.4873491e-02
_diffrn_orient_matrix_UB_32      -3.6601171e-02
_diffrn_orient_matrix_UB_33      4.6747878e-02
_diffrn_radiation_monochromator  'incoatec mirror optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5349
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.4698
_exptl_absorpt_correction_T_min  0.3964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1136.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0484P)²+1.4174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                5319
_reflns_number_total             5349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101066w_si_001.cif
_cod_data_source_block           vana1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4063971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_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 0.08757(3) 0.047080(17) 0.01115(2) 0.01613(10) Uani 1 1 d . . .
H1 H 0.0697(12) 0.1038(8) -0.0559(11) 0.019(4) Uiso 1 1 d . . .
O1 O 0.35217(9) 0.03231(7) 0.45622(9) 0.0400(3) Uani 1 1 d . B .
N1 N -0.00283(8) 0.02564(6) 0.07485(8) 0.0171(2) Uani 1 1 d . . .
N2 N -0.00274(8) 0.06551(6) 0.15897(8) 0.0179(2) Uani 1 1 d . . .
N11 N 0.19191(9) 0.11967(6) 0.11571(8) 0.0186(2) Uani 1 1 d . . .
N21 N 0.23556(8) 0.01517(6) 0.06626(8) 0.0185(2) Uani 1 1 d . . .
C1 C 0.27751(10) 0.07833(7) 0.12285(9) 0.0189(3) Uani 1 1 d . . .
C2 C 0.40144(11) 0.09691(7) 0.17400(10) 0.0217(3) Uani 1 1 d . . .
C3 C 0.46046(11) 0.11511(7) 0.11127(11) 0.0260(3) Uani 1 1 d . . .
H3 H 0.4221 0.1150 0.0373 0.031 Uiso 1 1 calc R . .
C4 C 0.57516(12) 0.13333(8) 0.15729(13) 0.0308(3) Uani 1 1 d . . .
H4 H 0.6149 0.1466 0.1147 0.037 Uiso 1 1 calc R . .
C5 C 0.63196(12) 0.13222(8) 0.26493(13) 0.0344(4) Uani 1 1 d . . .
H5 H 0.7108 0.1440 0.2960 0.041 Uiso 1 1 calc R . .
C6 C 0.57388(12) 0.11395(8) 0.32724(12) 0.0329(3) Uani 1 1 d . . .
H6 H 0.6131 0.1131 0.4011 0.040 Uiso 1 1 calc R . .
C7 C 0.45803(12) 0.09681(7) 0.28201(11) 0.0264(3) Uani 1 1 d . . .
H7 H 0.4180 0.0851 0.3250 0.032 Uiso 1 1 calc R . .
C11 C 0.19123(11) 0.19877(7) 0.14098(10) 0.0225(3) Uani 1 1 d . . .
C12 C 0.06982(11) 0.22628(7) 0.07878(11) 0.0245(3) Uani 1 1 d . . .
H12A H 0.0546 0.2262 0.0040 0.037 Uiso 1 1 calc R . .
H12B H 0.0619 0.2763 0.1009 0.037 Uiso 1 1 calc R . .
H12C H 0.0153 0.1939 0.0916 0.037 Uiso 1 1 calc R . .
C13 C 0.27264(13) 0.24517(8) 0.10913(14) 0.0359(4) Uani 1 1 d . . .
H13A H 0.3516 0.2340 0.1554 0.054 Uiso 1 1 calc R . .
H13B H 0.2574 0.2974 0.1148 0.054 Uiso 1 1 calc R . .
H13C H 0.2610 0.2338 0.0368 0.054 Uiso 1 1 calc R . .
C14 C 0.21986(13) 0.20552(8) 0.25814(11) 0.0320(3) Uani 1 1 d . . .
H14A H 0.1689 0.1738 0.2771 0.048 Uiso 1 1 calc R . .
H14B H 0.2100 0.2566 0.2751 0.048 Uiso 1 1 calc R . .
H14C H 0.2991 0.1905 0.2974 0.048 Uiso 1 1 calc R . .
C21 C 0.29097(11) -0.05775(7) 0.10303(11) 0.0231(3) Uani 1 1 d . . .
C22 C 0.22277(11) -0.11796(7) 0.02853(11) 0.0271(3) Uani 1 1 d . . .
H22A H 0.1465 -0.1209 0.0297 0.041 Uiso 1 1 calc R . .
H22B H 0.2619 -0.1651 0.0505 0.041 Uiso 1 1 calc R . .
H22C H 0.2160 -0.1065 -0.0425 0.041 Uiso 1 1 calc R . .
C23 C 0.41244(12) -0.06037(8) 0.10558(14) 0.0354(4) Uani 1 1 d . . .
H23A H 0.4117 -0.0426 0.0388 0.053 Uiso 1 1 calc R . .
H23B H 0.4405 -0.1110 0.1171 0.053 Uiso 1 1 calc R . .
H23C H 0.4626 -0.0292 0.1625 0.053 Uiso 1 1 calc R . .
C24 C 0.29268(14) -0.07299(8) 0.21199(11) 0.0345(3) Uani 1 1 d . . .
H24A H 0.3339 -0.0335 0.2598 0.052 Uiso 1 1 calc R . .
H24B H 0.3309 -0.1199 0.2379 0.052 Uiso 1 1 calc R . .
H24C H 0.2143 -0.0752 0.2080 0.052 Uiso 1 1 calc R . .
C30 C -0.05286(10) 0.04219(7) 0.21818(9) 0.0182(3) Uani 1 1 d . . .
C31 C -0.05622(10) 0.09446(7) 0.29891(10) 0.0195(3) Uani 1 1 d . . .
C32 C -0.04790(11) 0.17027(7) 0.28657(11) 0.0239(3) Uani 1 1 d . . .
H32 H -0.0434 0.1887 0.2244 0.029 Uiso 1 1 calc R . .
C33 C -0.04619(12) 0.21884(8) 0.36395(12) 0.0279(3) Uani 1 1 d . . .
H33 H -0.0390 0.2700 0.3548 0.033 Uiso 1 1 calc R . .
C34 C -0.05483(11) 0.19338(8) 0.45451(11) 0.0283(3) Uani 1 1 d . . .
H34 H -0.0528 0.2268 0.5077 0.034 Uiso 1 1 calc R . .
C35 C -0.06645(11) 0.11876(8) 0.46641(10) 0.0265(3) Uani 1 1 d . . .
H35 H -0.0739 0.1010 0.5276 0.032 Uiso 1 1 calc R . .
C36 C -0.06737(11) 0.06967(7) 0.38975(10) 0.0222(3) Uani 1 1 d . . .
H36 H -0.0757 0.0186 0.3990 0.027 Uiso 1 1 calc R . .
C41 C -0.10363(11) -0.03187(7) 0.21686(9) 0.0187(3) Uani 1 1 d . . .
C42 C -0.03358(11) -0.09320(7) 0.25149(10) 0.0219(3) Uani 1 1 d . . .
H42 H 0.0466 -0.0881 0.2734 0.026 Uiso 1 1 calc R . .
C43 C -0.07976(12) -0.16176(7) 0.25431(10) 0.0256(3) Uani 1 1 d . . .
H43 H -0.0312 -0.2033 0.2778 0.031 Uiso 1 1 calc R . .
C44 C -0.19648(12) -0.16986(8) 0.22289(11) 0.0283(3) Uani 1 1 d . . .
H44 H -0.2282 -0.2168 0.2244 0.034 Uiso 1 1 calc R . .
C45 C -0.26669(12) -0.10897(8) 0.18925(11) 0.0286(3) Uani 1 1 d . . .
H45 H -0.3468 -0.1143 0.1676 0.034 Uiso 1 1 calc R . .
C46 C -0.22082(11) -0.04042(7) 0.18693(10) 0.0235(3) Uani 1 1 d . . .
H46 H -0.2696 0.0011 0.1648 0.028 Uiso 1 1 calc R . .
C50 C 0.23760(13) 0.04162(10) 0.44702(14) 0.0418(4) Uani 1 1 d . B .
H50A H 0.2099 -0.0039 0.4682 0.050 Uiso 1 1 calc R . .
H50B H 0.1871 0.0530 0.3738 0.050 Uiso 1 1 calc R . .
C51 C 0.23749(15) 0.10457(12) 0.51816(15) 0.0523(5) Uani 1 1 d . . .
H51A H 0.1788 0.1413 0.4794 0.063 Uiso 1 1 calc R A 1
H51B H 0.2212 0.0864 0.5779 0.063 Uiso 1 1 calc R A 1
C52A C 0.3491(3) 0.1366(3) 0.5542(4) 0.0374(14) Uani 0.470(9) 1 d P B 1
H52A H 0.3753 0.1512 0.6285 0.045 Uiso 0.470(9) 1 calc PR B 1
H52B H 0.3495 0.1804 0.5121 0.045 Uiso 0.470(9) 1 calc PR B 1
C52B C 0.3666(3) 0.1014(3) 0.6003(3) 0.0379(13) Uani 0.530(9) 1 d P B 2
H52C H 0.3939 0.1506 0.6299 0.045 Uiso 0.530(9) 1 calc PR B 2
H52D H 0.3753 0.0669 0.6581 0.045 Uiso 0.530(9) 1 calc PR B 2
C53 C 0.42500(15) 0.07631(11) 0.54038(16) 0.0514(5) Uani 1 1 d . . .
H53A H 0.4871 0.0977 0.5236 0.062 Uiso 1 1 calc R B 1
H53B H 0.4591 0.0467 0.6050 0.062 Uiso 1 1 calc R B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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 80.34(5) . 3
N1 Si1 N21 119.51(5) . .
N1 Si1 N21 106.95(5) 3 .
N1 Si1 N11 99.17(5) . .
N1 Si1 N11 174.20(5) 3 .
N21 Si1 N11 68.18(4) . .
N1 Si1 C1 115.27(5) . .
N1 Si1 C1 142.23(5) 3 .
N21 Si1 C1 35.29(4) . .
N11 Si1 C1 33.07(4) . .
N21 Si1 Si1 120.68(4) . 3
N11 Si1 Si1 140.04(3) . 3
C1 Si1 Si1 143.27(4) . 3
C53 O1 C50 108.78(13) . .
N2 N1 Si1 122.10(8) . .
N2 N1 Si1 137.88(8) . 3
Si1 N1 Si1 99.66(5) . 3
C30 N2 N1 122.09(10) . .
C1 N11 C11 128.92(11) . .
C1 N11 Si1 88.41(8) . .
C11 N11 Si1 137.69(8) . .
C1 N21 C21 121.34(10) . .
C1 N21 Si1 94.56(8) . .
C21 N21 Si1 134.06(8) . .
N11 C1 N21 108.32(11) . .
N11 C1 C2 127.27(11) . .
N21 C1 C2 124.16(11) . .
N11 C1 Si1 58.53(7) . .
N21 C1 Si1 50.15(6) . .
C2 C1 Si1 168.73(9) . .
C7 C2 C3 119.84(12) . .
C7 C2 C1 121.19(12) . .
C3 C2 C1 118.98(12) . .
C4 C3 C2 119.83(13) . .
C5 C4 C3 120.32(14) . .
C4 C5 C6 119.98(13) . .
C5 C6 C7 120.26(14) . .
C2 C7 C6 119.75(14) . .
N11 C11 C14 108.03(11) . .
N11 C11 C12 106.41(10) . .
C14 C11 C12 109.94(11) . .
N11 C11 C13 113.52(11) . .
C14 C11 C13 111.02(12) . .
C12 C11 C13 107.81(11) . .
N21 C21 C22 109.81(10) . .
N21 C21 C24 108.66(11) . .
C22 C21 C24 108.95(11) . .
N21 C21 C23 111.83(11) . .
C22 C21 C23 107.12(11) . .
C24 C21 C23 110.43(12) . .
N2 C30 C31 115.99(11) . .
N2 C30 C41 127.43(11) . .
C31 C30 C41 116.54(10) . .
C32 C31 C36 117.89(12) . .
C32 C31 C30 120.87(11) . .
C36 C31 C30 121.24(12) . .
C33 C32 C31 120.84(13) . .
C32 C33 C34 120.62(13) . .
C35 C34 C33 119.16(12) . .
C34 C35 C36 120.63(13) . .
C35 C36 C31 120.81(13) . .
C42 C41 C46 118.73(12) . .
C42 C41 C30 120.26(11) . .
C46 C41 C30 120.91(11) . .
C43 C42 C41 120.64(12) . .
C44 C43 C42 120.16(12) . .
C43 C44 C45 119.56(13) . .
C46 C45 C44 120.42(13) . .
C45 C46 C41 120.48(12) . .
O1 C50 C51 107.17(13) . .
C52A C51 C50 106.30(19) . .
C50 C51 C52B 100.09(18) . .
C51 C52A C53 104.7(3) . .
C53 C52B C51 103.1(2) . .
C52B C53 O1 110.30(19) . .
O1 C53 C52A 105.55(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N1 1.7521(10) .
Si1 N1 1.8269(10) 3
Si1 N21 1.8306(10) .
Si1 N11 2.0280(11) .
Si1 C1 2.3769(13) .
Si1 Si1 2.7353(6) 3
O1 C53 1.422(2) .
O1 C50 1.4259(19) .
N1 N2 1.3767(14) .
N1 Si1 1.8268(10) 3
N2 C30 1.2964(16) .
N11 C1 1.2974(16) .
N11 C11 1.4835(16) .
N21 C1 1.3776(16) .
N21 C21 1.4969(16) .
C1 C2 1.4952(17) .
C2 C7 1.3880(19) .
C2 C3 1.3979(19) .
C3 C4 1.3873(19) .
C4 C5 1.384(2) .
C5 C6 1.384(2) .
C6 C7 1.395(2) .
C11 C14 1.5287(19) .
C11 C12 1.5314(18) .
C11 C13 1.5329(19) .
C21 C22 1.5246(18) .
C21 C24 1.533(2) .
C21 C23 1.5364(19) .
C30 C31 1.4855(17) .
C30 C41 1.4930(17) .
C31 C32 1.4002(19) .
C31 C36 1.4008(18) .
C32 C33 1.3866(19) .
C33 C34 1.387(2) .
C34 C35 1.384(2) .
C35 C36 1.3880(19) .
C41 C42 1.3928(18) .
C41 C46 1.3938(18) .
C42 C43 1.3875(19) .
C43 C44 1.385(2) .
C44 C45 1.386(2) .
C45 C46 1.3842(19) .
C50 C51 1.515(3) .
C51 C52A 1.435(4) .
C51 C52B 1.594(4) .
C52A C53 1.525(4) .
C52B C53 1.396(4) .
