#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:30:06 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180224 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/10/7111010.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_7111010
loop_
_publ_author_name
'Gehrhus, Barbara'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Slootweg, J. Chris'
_publ_section_title
;
 The diverse reactions of the silylene Si[(NCH2But)2C6H4-1,2] with
 Li[Si(SiMe3)3](thf)3 and K[N(SiMe3)2]
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1427
_journal_paper_doi               10.1039/b003833o
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H44 K N3 Si3'
_chemical_formula_structural     'C22 H44 K N3 Si3'
_chemical_formula_sum            'C22 H44 K N3 Si3'
_chemical_formula_weight         473.97
_chemical_name_common            '[K{Me3SiNSi(SiMe3)(C6H4(NCH2tBu)2)}]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-01-18T09:38:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.759(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4645(4)
_cell_length_b                   12.7533(3)
_cell_length_c                   16.5858(3)
_cell_measurement_reflns_used    10046
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     2846.72(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20621
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         4.55
_exptl_absorpt_coefficient_mu    0.326
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0361P)²+1.2475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                5363
_reflns_number_total             6689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003833osup1.cif
_cod_data_source_block           gerhus-3a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7111010
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
K K 0.14060(3) 0.96416(3) 0.25913(3) 0.03950(12) Uani 1 1 d .
Si1 Si 0.07164(3) 0.71839(3) 0.23769(2) 0.01866(10) Uani 1 1 d .
Si2 Si 0.00988(4) 0.55003(3) 0.20523(3) 0.02749(12) Uani 1 1 d .
Si3 Si -0.12226(3) 0.85611(3) 0.23040(3) 0.02323(11) Uani 1 1 d .
N1 N 0.15214(9) 0.70848(10) 0.32572(7) 0.0217(3) Uani 1 1 d .
N2 N 0.18089(9) 0.73475(10) 0.17866(7) 0.0205(3) Uani 1 1 d .
N3 N -0.00309(10) 0.81894(10) 0.23779(8) 0.0227(3) Uani 1 1 d .
C1 C 0.25134(11) 0.69734(11) 0.30699(9) 0.0216(3) Uani 1 1 d .
C2 C 0.26822(11) 0.71377(11) 0.22332(9) 0.0206(3) Uani 1 1 d .
C3 C 0.36466(12) 0.70846(13) 0.19556(10) 0.0270(3) Uani 1 1 d .
H3 H 0.3764 0.72 0.1401 0.032 Uiso 1 1 calc R
C4 C 0.44466(13) 0.68619(14) 0.24906(11) 0.0317(4) Uani 1 1 d .
H4 H 0.5104 0.6841 0.2299 0.038 Uiso 1 1 calc R
C5 C 0.42807(13) 0.66735(13) 0.32942(11) 0.0313(4) Uani 1 1 d .
H5 H 0.4824 0.6513 0.3652 0.038 Uiso 1 1 calc R
C6 C 0.33157(12) 0.67180(13) 0.35858(10) 0.0273(3) Uani 1 1 d .
H6 H 0.3207 0.6573 0.4138 0.033 Uiso 1 1 calc R
C7 C 0.11848(13) 0.67750(14) 0.40582(9) 0.0287(4) Uani 1 1 d .
H7A H 0.1651 0.6238 0.4277 0.034 Uiso 1 1 calc R
H7B H 0.0528 0.6434 0.3985 0.034 Uiso 1 1 calc R
C8 C 0.10905(14) 0.76395(16) 0.47004(10) 0.0356(4) Uani 1 1 d .
C9 C 0.02161(16) 0.83548(18) 0.44776(12) 0.0493(5) Uani 1 1 d .
H9A H -0.039 0.7934 0.441 0.074 Uiso 1 1 calc R
H9B H 0.0347 0.872 0.3972 0.074 Uiso 1 1 calc R
H9C H 0.0129 0.887 0.4908 0.074 Uiso 1 1 calc R
C10 C 0.08685(17) 0.7083(2) 0.54975(12) 0.0569(7) Uani 1 1 d .
H10A H 0.0262 0.6664 0.5428 0.085 Uiso 1 1 calc R
H10B H 0.0776 0.7607 0.5921 0.085 Uiso 1 1 calc R
H10C H 0.1426 0.6623 0.5652 0.085 Uiso 1 1 calc R
C11 C 0.20330(17) 0.82847(19) 0.48087(13) 0.0508(5) Uani 1 1 d .
H11A H 0.2591 0.7821 0.4952 0.076 Uiso 1 1 calc R
H11B H 0.1948 0.8799 0.524 0.076 Uiso 1 1 calc R
H11C H 0.2168 0.865 0.4304 0.076 Uiso 1 1 calc R
C12 C 0.17922(12) 0.71686(12) 0.09107(9) 0.0243(3) Uani 1 1 d .
H12A H 0.119 0.6755 0.0768 0.029 Uiso 1 1 calc R
H12B H 0.2374 0.6729 0.0786 0.029 Uiso 1 1 calc R
C13 C 0.18025(13) 0.81364(13) 0.03564(9) 0.0269(3) Uani 1 1 d .
C14 C 0.08332(14) 0.87500(15) 0.04316(10) 0.0361(4) Uani 1 1 d .
H14A H 0.0268 0.8286 0.0309 0.054 Uiso 1 1 calc R
H14B H 0.0823 0.9338 0.0051 0.054 Uiso 1 1 calc R
H14C H 0.0787 0.9019 0.0983 0.054 Uiso 1 1 calc R
C15 C 0.18690(16) 0.77285(16) -0.05111(10) 0.0411(5) Uani 1 1 d .
H15A H 0.1302 0.7268 -0.0636 0.062 Uiso 1 1 calc R
H15B H 0.2488 0.7335 -0.0565 0.062 Uiso 1 1 calc R
H15C H 0.1859 0.8322 -0.0886 0.062 Uiso 1 1 calc R
C16 C 0.26859(15) 0.88480(15) 0.05455(12) 0.0407(5) Uani 1 1 d .
H16A H 0.3303 0.845 0.0495 0.061 Uiso 1 1 calc R
H16B H 0.2644 0.9115 0.1097 0.061 Uiso 1 1 calc R
H16C H 0.2679 0.9437 0.0166 0.061 Uiso 1 1 calc R
C17 C 0.12238(15) 0.46476(15) 0.19205(15) 0.0484(5) Uani 1 1 d .
H17A H 0.164 0.4661 0.2416 0.073 Uiso 1 1 calc R
H17B H 0.1606 0.4912 0.147 0.073 Uiso 1 1 calc R
H17C H 0.1011 0.3926 0.1807 0.073 Uiso 1 1 calc R
C18 C -0.06219(16) 0.48891(16) 0.28780(13) 0.0455(5) Uani 1 1 d .
H18A H -0.0225 0.4909 0.3383 0.068 Uiso 1 1 calc R
H18B H -0.0777 0.4159 0.2738 0.068 Uiso 1 1 calc R
H18C H -0.1241 0.5279 0.2945 0.068 Uiso 1 1 calc R
C19 C -0.06770(16) 0.54555(17) 0.10913(12) 0.0451(5) Uani 1 1 d .
H19A H -0.0307 0.5773 0.0654 0.068 Uiso 1 1 calc R
H19B H -0.1295 0.5845 0.1163 0.068 Uiso 1 1 calc R
H19C H -0.0833 0.4725 0.0955 0.068 Uiso 1 1 calc R
C20 C -0.15237(15) 0.95692(15) 0.30934(13) 0.0418(5) Uani 1 1 d .
H20A H -0.1055 1.0155 0.3065 0.063 Uiso 1 1 calc R
H20B H -0.1471 0.9248 0.363 0.063 Uiso 1 1 calc R
H20C H -0.2202 0.9828 0.2995 0.063 Uiso 1 1 calc R
C21 C -0.21584(13) 0.74839(15) 0.24077(12) 0.0354(4) Uani 1 1 d .
H21A H -0.2031 0.7112 0.2917 0.053 Uiso 1 1 calc R
H21B H -0.2105 0.6993 0.1957 0.053 Uiso 1 1 calc R
H21C H -0.2828 0.7785 0.2403 0.053 Uiso 1 1 calc R
C22 C -0.15254(14) 0.92271(17) 0.13149(12) 0.0428(5) Uani 1 1 d .
H22A H -0.1053 0.9799 0.1232 0.064 Uiso 1 1 calc R
H22B H -0.2201 0.9512 0.1322 0.064 Uiso 1 1 calc R
H22C H -0.148 0.8718 0.0875 0.064 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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_3
N3 Si1 N1 114.31(6) .
N3 Si1 N2 115.04(6) .
N1 Si1 N2 88.15(6) .
N3 Si1 Si2 120.20(5) .
N1 Si1 Si2 108.74(5) .
N2 Si1 Si2 105.61(5) .
N3 Si1 K 54.67(5) .
N1 Si1 K 79.49(4) .
N2 Si1 K 73.50(4) .
Si2 Si1 K 171.75(2) .
C18 Si2 C19 108.70(10) .
C18 Si2 C17 106.34(10) .
C19 Si2 C17 108.19(11) .
C18 Si2 Si1 113.51(7) .
C19 Si2 Si1 113.83(7) .
C17 Si2 Si1 105.84(7) .
N3 Si3 C21 115.53(7) .
N3 Si3 C22 111.92(8) .
C21 Si3 C22 106.41(9) .
N3 Si3 C20 111.58(8) .
C21 Si3 C20 106.02(9) .
C22 Si3 C20 104.59(10) .
C1 N1 C7 120.00(12) .
C1 N1 Si1 112.72(10) .
C7 N1 Si1 123.93(10) .
C2 N2 C12 118.80(13) .
C2 N2 Si1 112.17(10) .
C12 N2 Si1 122.03(10) .
Si1 N3 Si3 144.40(9) .
Si1 N3 K 95.74(6) .
Si3 N3 K 119.86(6) .
N1 C1 C6 128.23(14) .
N1 C1 C2 112.66(13) .
C6 C1 C2 119.11(14) .
C3 C2 N2 127.77(14) .
C3 C2 C1 119.46(14) .
N2 C2 C1 112.77(13) .
C2 C3 C4 120.41(15) .
C5 C4 C3 120.15(16) .
C5 C4 K 79.04(10) 2_545
C3 C4 K 83.08(10) 2_545
C4 C5 C6 120.38(15) .
C4 C5 K 75.11(10) 2_545
C6 C5 K 86.06(10) 2_545
C1 C6 C5 120.42(15) .
N1 C7 C8 117.80(14) .
C11 C8 C9 109.91(18) .
C11 C8 C10 109.41(17) .
C9 C8 C10 108.38(16) .
C11 C8 C7 112.54(15) .
C9 C8 C7 109.86(15) .
C10 C8 C7 106.62(17) .
N2 C12 C13 117.76(13) .
C16 C13 C14 109.97(16) .
C16 C13 C15 109.12(15) .
C14 C13 C15 108.92(14) .
C16 C13 C12 112.12(14) .
C14 C13 C12 109.76(13) .
C15 C13 C12 106.86(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K N3 2.6938(14) .
Si1 N3 1.6302(13) .
Si1 N1 1.7959(13) .
Si1 N2 1.8040(13) .
Si1 Si2 2.3588(6) .
Si2 C18 1.873(2) .
Si2 C19 1.880(2) .
Si2 C17 1.883(2) .
Si3 N3 1.6739(14) .
Si3 C21 1.8757(18) .
Si3 C22 1.8809(18) .
Si3 C20 1.8878(19) .
N1 C1 1.388(2) .
N1 C7 1.4709(19) .
N2 C2 1.3962(19) .
N2 C12 1.4700(19) .
C1 C6 1.396(2) .
C1 C2 1.429(2) .
C2 C3 1.393(2) .
C3 C4 1.403(2) .
C4 C5 1.379(3) .
C4 K 3.0569(18) 2_545
C5 C6 1.401(2) .
C5 K 3.1054(18) 2_545
C7 C8 1.541(2) .
C8 C11 1.518(3) .
C8 C9 1.526(3) .
C8 C10 1.538(3) .
C12 C13 1.539(2) .
C13 C16 1.521(3) .
C13 C14 1.530(2) .
C13 C15 1.535(2) .
