#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027563.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_7027563
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_sum            'C11 H30 K N Si3'
_chemical_formula_weight         299.73
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.586(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4021(9)
_cell_length_b                   14.6824(14)
_cell_length_c                   12.7646(12)
_cell_measurement_reflns_used    11716
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.11
_cell_volume                     1760.3(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13832
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.8206
_exptl_absorpt_correction_T_min  0.9011
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         0.033
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0378P)²+0.6798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0751
_refine_ls_wR_factor_obs         0.0728
_reflns_number_observed          3740
_reflns_number_total             4042
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904043Isup1.cif
_cod_data_source_block           ki5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.6798P] 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^)+(0.0378P)^2^+0.6798P] 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      p2(1)/c
_cod_database_code               7027563
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
K1 K 0.79375(3) 0.75341(2) 1.09037(2) 0.03068(9) Uani 1 d .
Si1 Si 0.70980(4) 0.62761(2) 0.85653(3) 0.02098(9) Uani 1 d .
Si2 Si 0.65328(3) 0.83378(2) 0.82200(3) 0.02093(9) Uani 1 d .
Si3 Si 0.97340(3) 0.75526(2) 0.84865(3) 0.02104(9) Uani 1 d .
C1 C 0.78208(12) 0.74208(8) 0.84079(9) 0.0197(2) Uani 1 d .
C2 C 0.81361(18) 0.54973(11) 0.95072(13) 0.0408(4) Uani 1 d .
H2A H 0.8640 0.5864 1.0047 0.049 Uiso 1 calc R
H2B H 0.8826 0.5145 0.9121 0.049 Uiso 1 calc R
H2C H 0.7478 0.5081 0.9839 0.049 Uiso 1 calc R
C3 C 0.69286(18) 0.55935(10) 0.73104(11) 0.0348(3) Uani 1 d .
H3A H 0.6212 0.5875 0.6832 0.042 Uiso 1 calc R
H3B H 0.6638 0.4970 0.7470 0.042 Uiso 1 calc R
H3C H 0.7848 0.5582 0.6978 0.042 Uiso 1 calc R
C4 C 0.52520(16) 0.62406(11) 0.90889(14) 0.0403(4) Uani 1 d .
H4A H 0.5266(3) 0.6513(8) 0.9753(8) 0.048 Uiso 1 calc R
H4B H 0.4955(6) 0.5634(7) 0.9141(9) 0.048 Uiso 1 calc R
H4C H 0.4620(8) 0.6557(8) 0.8632(7) 0.048 Uiso 1 calc R
C5 C 0.50018(15) 0.80411(11) 0.72588(11) 0.0351(3) Uani 1 d .
H5A H 0.4096 0.8174 0.7578 0.042 Uiso 1 calc R
H5B H 0.5044 0.7392 0.7083 0.042 Uiso 1 calc R
H5C H 0.5075 0.8404 0.6619 0.042 Uiso 1 calc R
C6 C 0.72331(17) 0.94462(10) 0.77015(13) 0.0388(3) Uani 1 d .
H6A H 0.6476(9) 0.9884(5) 0.7648(8) 0.047 Uiso 1 calc R
H6B H 0.7602(12) 0.9348(2) 0.7022(8) 0.047 Uiso 1 calc R
H6C H 0.7978(12) 0.9671(5) 0.8171(7) 0.047 Uiso 1 calc R
C7 C 0.56427(15) 0.87288(10) 0.94431(11) 0.0308(3) Uani 1 d .
H7A H 0.6339 0.9047 0.9906 0.037 Uiso 1 calc R
H7B H 0.5271 0.8199 0.9809 0.037 Uiso 1 calc R
H7C H 0.4858 0.9143 0.9247 0.037 Uiso 1 calc R
C8 C 1.07536(15) 0.64792(11) 0.82181(13) 0.0375(3) Uani 1 d .
H8A H 1.1709(11) 0.66321(19) 0.8054(9) 0.045 Uiso 1 calc R
H8B H 1.0300(8) 0.6163(5) 0.7638(8) 0.045 Uiso 1 calc R
H8C H 1.0770(10) 0.6096(5) 0.8826(7) 0.045 Uiso 1 calc R
C9 C 1.04897(15) 0.84045(11) 0.75433(12) 0.0342(3) Uani 1 d .
H9A H 0.9973 0.8982 0.7587 0.041 Uiso 1 calc R
H9B H 1.0386 0.8167 0.6827 0.041 Uiso 1 calc R
H9C H 1.1500 0.8505 0.7728 0.041 Uiso 1 calc R
C10 C 1.01235(19) 0.88672(11) 0.99727(13) 0.0406(3) Uani 1 d .
H10A H 1.0259 0.8981 1.0727 0.049 Uiso 1 calc R
H10B H 0.9142 0.9017 0.9744 0.049 Uiso 1 calc R
H10C H 1.0784 0.9247 0.9592 0.049 Uiso 1 calc R
C11 C 1.18902(16) 0.76992(15) 1.00540(14) 0.0482(4) Uani 1 d .
H11A H 1.2522(8) 0.8042(8) 0.9598(8) 0.058 Uiso 1 calc R
H11B H 1.2059(4) 0.7039(8) 0.9972(10) 0.058 Uiso 1 calc R
H11C H 1.2093(5) 0.7876(8) 1.0793(9) 0.058 Uiso 1 calc R
N1 N 1.04004(11) 0.79077(8) 0.97566(9) 0.0280(2) Uani 1 d .
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
N1 K1 C10 27.93(4) . .
N1 K1 C1 59.22(3) . .
C10 K1 C1 69.19(4) . .
N1 K1 C1 125.04(3) . 4_576
C10 K1 C1 114.89(4) . 4_576
C1 K1 C1 175.67(4) . 4_576
N1 K1 C7 97.67(4) . .
C10 K1 C7 82.87(4) . .
C1 K1 C7 57.98(3) . .
C1 K1 C7 120.18(3) 4_576 .
N1 K1 C9 80.04(4) . 4_576
C10 K1 C9 91.72(4) . 4_576
C1 K1 C9 125.81(3) . 4_576
C1 K1 C9 56.62(3) 4_576 4_576
C7 K1 C9 171.70(4) . 4_576
C1 Si1 C4 114.61(6) . .
C1 Si1 C3 114.34(6) . .
C4 Si1 C3 103.99(7) . .
C1 Si1 C2 116.15(7) . .
C4 Si1 C2 102.35(8) . .
C3 Si1 C2 103.81(7) . .
C1 Sy1 K1 63.03(4) . .
C4 Si1 K1 83.?0(5) . .
C3 Si1 K1 172.06(5) . .
C2 Si1 K1 72.17(6) . .
C1 Si1 K1 53.58(4) . 4_575
C4 Si1 K1 122.79(6) . 4_575
C3 Si1 K1 61.04(5) . 4_575
C2 Si1 K1 134.25(6) . 4_575
K1 Si1 K1 116.577(11) . 4_575
C1 Si2 C6 116.34(6) . .
C1 Si2 C7 115.59(6) . .
C6 Si2 C7 101.65(7) . .
C1 Si2 C5 113.32(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 N1 2.8484(12) .
K1 C10 3.1126(17) .
K1 C1 3.1870(12) .
K1 C1 3.2041(13) 4_576
K1 C7 3.2932(14) .
K1 C9 3.4036(16) 4_576
Si1 C1 1.8274(12) .
Si1 C4 1.8886(15) .
Si1 C3 1.8901(14) .
Si1 C2 1.8973(15) .
Si1 K1 3.9319(5) 4_575
Si2 C1 1.8195(12) .
Si2 C6 1.8866(15) .
Si2 C7 1.8934(14) .
Si2 C5 1.8994(14) .
Si2 K1 3.5324(5) 4_575
Si3 N1 1.7892(12) .
Si3 C1 1.8075(12) .
Si3 C8 1.8840(15) .
Si3 C9 1.8963(14) .
Si3 K1 3.6382(5) 4_575
C1 K1 3.2041(13) 4_575
C10 N1 1.461(2) .
C11 N1 1.4670(18) .
