#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027562.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_7027562
loop_
_publ_author_name
'Al-Juaid, Salih S.'
'Eaborn, Colin'
'El-Hamruni, Salima'
'Farook, Adam'
'Hitchcock, Peter B.'
'Hopman, Martijn'
'Smith, J. David'
'Clegg, William'
'Izod, Keith'
'O’Shaughnessy, Paul'
_publ_section_title
;
 Tris(triorganosilyl)methyl derivatives of potassium and lithium bearing
 dimethylamino or methoxy substituents at silicon. Crystal structures of
 KC(SiMe3)2(SiMe2NMe2), KC(SiMe2NMe2)3 and [LiC(SiMe3)(SiMe2OMe)2]2
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3267
_journal_paper_doi               10.1039/a904043i
_journal_year                    1999
_chemical_formula_structural     '[K{C(SiMe2NMe2)3}]n'
_chemical_formula_sum            'C13 H36 K N3 Si3'
_chemical_formula_weight         357.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.219(5)
_cell_length_b                   9.486(2)
_cell_length_c                   13.656(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2071.2(10)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1881
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.427
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.196
_refine_ls_goodness_of_fit_obs   1.198
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1877
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.309
_refine_ls_restrained_S_obs      1.197
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_obs          0.0398
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0454P)²+6.3977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1316
_refine_ls_wR_factor_obs         0.1182
_reflns_number_observed          1818
_reflns_number_total             1881
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904043Isup1.cif
_cod_data_source_block           aug597
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+6.3977P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+6.3977P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7027562
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
K K 0.75856(8) 1.04805(14) 0.67279(9) 0.0315(3) Uani 1 d .
Si1 Si 0.75254(10) 0.66789(15) 0.34978(11) 0.0212(3) Uani 1 d .
Si2 Si 0.83065(9) 0.9549(2) 0.42441(11) 0.0204(3) Uani 1 d .
Si3 Si 0.63906(9) 0.9103(2) 0.41923(10) 0.0191(3) Uani 1 d .
N1 N 0.7599(4) 0.6627(6) 0.2209(4) 0.0321(12) Uani 1 d .
N2 N 0.8750(3) 0.9586(6) 0.5536(4) 0.0316(12) Uani 1 d .
N3 N 0.6326(3) 0.8994(5) 0.5477(4) 0.0255(11) Uani 1 d .
C1 C 0.7376(3) 0.8471(5) 0.3917(4) 0.0180(11) Uani 1 d .
C2 C 0.6691(4) 0.5342(7) 0.3663(6) 0.038(2) Uani 1 d .
H2C H 0.6837(4) 0.4423(7) 0.3413(6) 0.056 Uiso 1 calc R
H2B H 0.6150(4) 0.5650(7) 0.3292(6) 0.056 Uiso 1 calc R
H2A H 0.6652(4) 0.5262(7) 0.4369(6) 0.056 Uiso 1 calc R
C3 C 0.8495(4) 0.5758(7) 0.4132(5) 0.0318(14) Uani 1 d .
H3C H 0.8518(4) 0.4808(7) 0.3856(5) 0.048 Uiso 1 calc R
H3B H 0.8483(4) 0.5694(7) 0.4846(5) 0.048 Uiso 1 calc R
H3A H 0.8989(4) 0.6292(7) 0.4025(5) 0.048 Uiso 1 calc R
C4 C 0.8209(7) 0.5709(9) 0.1848(7) 0.059(2) Uani 1 d .
H4C H 0.8743(7) 0.5753(9) 0.2307(7) 0.089 Uiso 1 calc R
H4B H 0.8291(7) 0.6022(9) 0.1188(7) 0.089 Uiso 1 calc R
H4A H 0.8002(7) 0.4736(9) 0.1809(7) 0.089 Uiso 1 calc R
C5 C 0.6807(6) 0.6560(8) 0.1527(5) 0.050(2) Uani 1 d .
H5C H 0.6398(6) 0.7174(8) 0.1767(5) 0.076 Uiso 1 calc R
H5B H 0.6600(6) 0.5587(8) 0.1487(5) 0.076 Uiso 1 calc R
H5A H 0.6890(6) 0.6873(8) 0.0866(5) 0.076 Uiso 1 calc R
C6 C 0.9193(4) 0.9019(7) 0.3568(5) 0.0298(13) Uani 1 d .
H6C H 0.9675(4) 0.9636(7) 0.3775(5) 0.045 Uiso 1 calc R
H6B H 0.9008(4) 0.9107(7) 0.2849(5) 0.045 Uiso 1 calc R
H6A H 0.9353(4) 0.8039(7) 0.3730(5) 0.045 Uiso 1 calc R
C7 C 0.8165(4) 1.1492(7) 0.3940(6) 0.038(2) Uani 1 d .
H7C H 0.8697(4) 1.1985(7) 0.4142(6) 0.057 Uiso 1 calc R
H7B H 0.7742(4) 1.1888(7) 0.4297(6) 0.057 Uiso 1 calc R
H7A H 0.7981(4) 1.1608(7) 0.3224(6) 0.057 Uiso 1 calc R
C8 C 0.8913(5) 0.8272(9) 0.6038(5) 0.043(2) Uani 1 d .
H8C H 0.8422(5) 0.7658(9) 0.5877(5) 0.065 Uiso 1 calc R
H8B H 0.9030(5) 0.8434(9) 0.6757(5) 0.065 Uiso 1 calc R
H8A H 0.9397(5) 0.7820(9) 0.5827(5) 0.065 Uiso 1 calc R
C9 C 0.9492(5) 1.0496(10) 0.5787(6) 0.054(2) Uani 1 d .
H9C H 0.9387(5) 1.1403(10) 0.5445(6) 0.081 Uiso 1 calc R
H9B H 0.9975(5) 1.0037(10) 0.5576(6) 0.081 Uiso 1 calc R
H9A H 0.9609(5) 1.0652(10) 0.6506(6) 0.081 Uiso 1 calc R
C10 C 0.5423(4) 0.8172(7) 0.3518(5) 0.035(2) Uani 1 d .
H10C H 0.4923(4) 0.8588(7) 0.3716(5) 0.052 Uiso 1 calc R
H10B H 0.5452(4) 0.7168(7) 0.3690(5) 0.052 Uiso 1 calc R
H10A H 0.5395(4) 0.8279(7) 0.2799(5) 0.052 Uiso 1 calc R
C11 C 0.6152(4) 1.1029(6) 0.3897(5) 0.0299(13) Uani 1 d .
H11C H 0.5607(4) 1.1270(6) 0.4071(5) 0.045 Uiso 1 calc R
H11B H 0.6139(4) 1.1193(6) 0.3186(5) 0.045 Uiso 1 calc R
H11A H 0.6586(4) 1.1619(6) 0.4281(5) 0.045 Uiso 1 calc R
C12 C 0.6519(4) 0.7621(7) 0.5942(5) 0.0339(15) Uani 1 d .
H12C H 0.7021(4) 0.7235(7) 0.5731(5) 0.051 Uiso 1 calc R
H12B H 0.6048(4) 0.6978(7) 0.5741(5) 0.051 Uiso 1 calc R
H12A H 0.6617(4) 0.7728(7) 0.6666(5) 0.051 Uiso 1 calc R
C13 C 0.5574(5) 0.9586(8) 0.5786(5) 0.041(2) Uani 1 d .
H13C H 0.5450(5) 1.0506(8) 0.5471(5) 0.062 Uiso 1 calc R
H13B H 0.5669(5) 0.9697(8) 0.6510(5) 0.062 Uiso 1 calc R
H13A H 0.5100(5) 0.8948(8) 0.5585(5) 0.062 Uiso 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'
K K 0.2009 0.2494 '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
N3 K N1 127.3(2) . 2_575
N3 K N2 89.27(15) . .
N1 K N2 116.5(2) 2_575 .
N3 K Si2 133.90(11) . 2_575
N1 K Si2 77.71(11) 2_575 2_575
N2 K Si2 115.19(12) . 2_575
N1 Si1 C1 111.7(2) . .
N1 Si1 C3 104.6(3) . .
C1 Si1 C3 115.7(3) . .
N1 Si1 C2 105.4(3) . .
C1 Si1 C2 116.8(3) . .
C3 Si1 C2 101.1(3) . .
N2 Si2 C1 115.7(3) . .
N2 Si2 C7 102.1(3) . .
C1 Si2 C7 115.4(3) . .
N2 Si2 C6 105.8(3) . .
C1 Si2 C6 113.4(3) . .
C7 Si2 C6 103.0(3) . .
N2 Si2 K 176.2(2) . 2_574
C1 Si2 K 67.7(2) . 2_574
C7 Si2 K 77.3(2) . 2_574
C6 Si2 K 70.8(2) . 2_574
N3 Si3 C1 112.8(2) . .
N3 Si3 C11 102.8(3) . .
C1 Si3 C11 115.6(3) . .
N3 Si3 C10 105.7(3) . .
C1 Si3 C10 115.7(3) . .
C11 Si3 C10 102.8(3) . .
C5 N1 C4 109.4(6) . .
C5 N1 Si1 115.7(5) . .
C4 N1 Si1 120.6(5) . .
C5 N1 K 85.5(4) . 2_574
C4 N1 K 118.7(5) . 2_574
Si1 N1 K 101.7(2) . 2_574
C8 N2 C9 108.8(6) . .
C8 N2 Si2 117.9(4) . .
C9 N2 Si2 114.7(5) . .
C8 N2 K 94.2(4) . .
C9 N2 K 106.8(4) . .
Si2 N2 K 112.2(2) . .
C12 N3 C13 110.1(5) . .
C12 N3 Si3 115.9(4) . .
C13 N3 Si3 116.9(4) . .
C12 N3 K 95.9(4) . .
C13 N3 K 100.8(4) . .
Si3 N3 K 114.4(2) . .
Si3 C1 Si2 119.4(3) . .
Si3 C1 Si1 122.9(3) . .
Si2 C1 Si1 117.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K N3 2.812(5) .
K N1 2.821(6) 2_575
K N2 2.823(5) .
K Si2 3.439(2) 2_575
Si1 N1 1.785(5) .
Si1 C1 1.823(5) .
Si1 C3 1.879(7) .
Si1 C2 1.896(7) .
Si2 N2 1.790(5) .
Si2 C1 1.815(5) .
Si2 C7 1.895(7) .
Si2 C6 1.903(6) .
Si2 K 3.439(2) 2_574
Si3 N3 1.778(5) .
Si3 C1 1.805(6) .
Si3 C11 1.898(6) .
Si3 C10 1.899(6) .
N1 C5 1.456(9) .
N1 C4 1.464(9) .
N1 K 2.821(5) 2_574
N2 C8 1.426(9) .
N2 C9 1.474(9) .
N3 C12 1.460(8) .
N3 C13 1.468(8) .
