#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:59:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180218 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/04/7110410.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_7110410
loop_
_publ_author_name
'Alder, Roger W.'
'Blake, Michael E.'
'Bortolotti, Christel'
'Bufali, Simone'
'Butts, Craig P.'
'Linehan, Emma'
'Oliva, Josep M.'
'Guy Orpen, A.'
'Quayle, Michael J.'
_publ_section_title
;
 Complexation of stable carbenes with alkali metals
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              241
_journal_paper_doi               10.1039/a808951e
_journal_year                    1999
_chemical_formula_sum            'C32 H76 K2 N6 Si4'
_chemical_formula_weight         735.55
_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
_cell_angle_alpha                73.97(2)
_cell_angle_beta                 73.132(12)
_cell_angle_gamma                69.426(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4128(12)
_cell_length_b                   10.937(3)
_cell_length_c                   12.306(2)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.75
_cell_volume                     1113.4(4)
_computing_cell_refinement       'SMART (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SMART (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11499
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.14
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.887862
_exptl_absorpt_correction_T_min  0.774504
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       'Irregular Block'
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.988
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_obs          0.0266
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0438P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0762
_refine_ls_wR_factor_obs         0.0743
_reflns_number_observed          4058
_reflns_number_total             5034
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808951esup1.cif
_cod_data_source_block           kcarb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] 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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1113.5(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110410
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
K1 K 0.11811(3) 0.97106(3) 0.11082(2) 0.02696(8) Uani 1 d .
Si1 Si 0.15997(4) 1.20943(4) -0.15326(3) 0.02235(9) Uani 1 d .
Si2 Si 0.15270(4) 0.70000(3) -0.01774(3) 0.02170(9) Uani 1 d .
N1 N 0.00112(12) 0.80333(10) 0.05429(9) 0.0226(2) Uani 1 d .
N2 N 0.25374(12) 0.95569(11) 0.38261(9) 0.0234(2) Uani 1 d .
N6 N 0.28142(12) 0.74025(11) 0.38040(9) 0.0231(2) Uani 1 d .
C1 C 0.23989(14) 0.86936(13) 0.32944(11) 0.0219(3) Uani 1 d .
C3 C 0.3157(2) 0.92015(14) 0.48752(13) 0.0324(3) Uani 1 d .
H3A H 0.2291(2) 0.92793(14) 0.55637(13) 0.039 Uiso 1 calc R
H3B H 0.3736(2) 0.98205(14) 0.48314(13) 0.039 Uiso 1 calc R
C4 C 0.4226(2) 0.77897(15) 0.49872(14) 0.0358(3) Uani 1 d .
H4A H 0.5186(2) 0.77468(15) 0.43753(14) 0.043 Uiso 1 calc R
H4B H 0.4521(2) 0.75011(15) 0.57485(14) 0.043 Uiso 1 calc R
C5 C 0.3411(2) 0.68798(14) 0.48748(12) 0.0305(3) Uani 1 d .
H5A H 0.4146(2) 0.59753(14) 0.48554(12) 0.037 Uiso 1 calc R
H5B H 0.2541(2) 0.68195(14) 0.55511(12) 0.037 Uiso 1 calc R
C7 C 0.2102(2) 1.09826(13) 0.32870(12) 0.0266(3) Uani 1 d .
H7A H 0.1501(2) 1.10905(13) 0.26995(12) 0.032 Uiso 1 calc R
C8 C 0.3510(2) 1.1450(2) 0.2645(2) 0.0512(5) Uani 1 d .
H8A H 0.4170(2) 1.0873(2) 0.2094(2) 0.077 Uiso 1 calc R
H8B H 0.4099(2) 1.1410(2) 0.3199(2) 0.077 Uiso 1 calc R
H8C H 0.3173(2) 1.2368(2) 0.2227(2) 0.077 Uiso 1 calc R
C9 C 0.1042(2) 1.1842(2) 0.41530(14) 0.0410(4) Uani 1 d .
H9A H 0.0144(2) 1.1514(2) 0.45527(14) 0.062 Uiso 1 calc R
H9B H 0.0684(2) 1.2765(2) 0.37472(14) 0.062 Uiso 1 calc R
H9C H 0.1610(2) 1.1806(2) 0.47196(14) 0.062 Uiso 1 calc R
C10 C 0.27172(15) 0.64107(13) 0.32456(12) 0.0249(3) Uani 1 d .
H10A H 0.21368(15) 0.69107(13) 0.26158(12) 0.030 Uiso 1 calc R
C11 C 0.1806(2) 0.5496(2) 0.40849(14) 0.0373(3) Uani 1 d .
H11A H 0.0781(2) 0.6033(2) 0.44336(14) 0.056 Uiso 1 calc R
H11B H 0.2371(2) 0.4956(2) 0.46944(14) 0.056 Uiso 1 calc R
H11C H 0.1679(2) 0.4911(2) 0.36664(14) 0.056 Uiso 1 calc R
C12 C 0.4328(2) 0.56164(15) 0.26781(13) 0.0331(3) Uani 1 d .
H12A H 0.4884(2) 0.62308(15) 0.21447(13) 0.050 Uiso 1 calc R
H12B H 0.4221(2) 0.50321(15) 0.22489(13) 0.050 Uiso 1 calc R
H12C H 0.4912(2) 0.50770(15) 0.32767(13) 0.050 Uiso 1 calc R
C13 C 0.3405(2) 1.1487(2) -0.09110(13) 0.0349(3) Uani 1 d .
H13A H 0.4300(3) 1.1609(10) -0.1532(2) 0.052 Uiso 1 calc R
H13B H 0.3592(7) 1.0541(3) -0.0555(8) 0.052 Uiso 1 calc R
H13C H 0.3256(5) 1.1997(7) -0.0325(7) 0.052 Uiso 1 calc R
C14 C 0.2035(2) 1.1024(2) -0.26326(13) 0.0354(3) Uani 1 d .
H14A H 0.2992(7) 1.1098(8) -0.3200(5) 0.053 Uiso 1 calc R
H14B H 0.1172(6) 1.1327(7) -0.3030(6) 0.053 Uiso 1 calc R
H14C H 0.2166(12) 1.0094(2) -0.2237(2) 0.053 Uiso 1 calc R
C15 C 0.1606(2) 1.38010(15) -0.24177(13) 0.0348(3) Uani 1 d .
H15A H 0.1386(2) 1.44141(15) -0.19000(13) 0.052 Uiso 1 calc R
H15B H 0.0807(2) 1.41225(15) -0.28779(13) 0.052 Uiso 1 calc R
H15C H 0.2627(2) 1.37537(15) -0.29354(13) 0.052 Uiso 1 calc R
C16 C 0.3400(2) 0.73803(15) -0.03395(13) 0.0331(3) Uani 1 d .
H16A H 0.4264(2) 0.6764(7) -0.0772(8) 0.050 Uiso 1 calc R
H16B H 0.3587(6) 0.7276(10) 0.04284(13) 0.050 Uiso 1 calc R
H16C H 0.3317(5) 0.8297(4) -0.0759(8) 0.050 Uiso 1 calc R
C17 C 0.1397(2) 0.71672(14) -0.17202(12) 0.0323(3) Uani 1 d .
H17A H 0.1185(2) 0.81059(14) -0.21048(12) 0.048 Uiso 1 calc R
H17B H 0.0556(2) 0.68344(14) -0.17185(12) 0.048 Uiso 1 calc R
H17C H 0.2383(2) 0.66478(14) -0.21365(12) 0.048 Uiso 1 calc R
C18 C 0.1934(2) 0.51677(14) 0.04708(13) 0.0326(3) Uani 1 d .
H18A H 0.2015(2) 0.50179(14) 0.12763(13) 0.049 Uiso 1 calc R
H18B H 0.2914(2) 0.46731(14) 0.00275(13) 0.049 Uiso 1 calc R
H18C H 0.1087(2) 0.48597(14) 0.04455(13) 0.049 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
N1 K1 N1 94.95(3) . 2_575
N1 K1 C1 116.03(4) . .
N1 K1 C1 146.92(4) 2_575 .
N1 K1 K1 48.38(3) . 2_575
N1 K1 K1 46.57(3) 2_575 2_575
C1 K1 K1 161.54(3) . 2_575
N1 Si1 C15 117.24(6) 2_575 .
N1 Si1 C14 110.45(6) 2_575 .
C15 Si1 C14 104.92(7) . .
N1 Si1 C13 113.67(6) 2_575 .
C15 Si1 C13 104.46(7) . .
C14 Si1 C13 105.04(7) . .
N1 Si2 C18 116.85(6) . .
N1 Si2 C17 113.03(6) . .
C18 Si2 C17 105.70(7) . .
N1 Si2 C16 111.44(6) . .
C18 Si2 C16 104.84(7) . .
C17 Si2 C16 103.85(7) . .
Si2 N1 Si1 136.04(7) . 2_575
Si2 N1 K1 106.35(5) . .
Si1 N1 K1 108.16(5) 2_575 .
Si2 N1 K1 107.52(5) . 2_575
Si1 N1 K1 101.82(5) 2_575 2_575
K1 N1 K1 85.05(3) . 2_575
C1 N2 C3 125.73(11) . .
C1 N2 C7 117.79(10) . .
C3 N2 C7 116.42(11) . .
C1 N6 C5 125.01(11) . .
C1 N6 C10 118.55(10) . .
C5 N6 C10 116.42(10) . .
N6 C1 N2 116.26(11) . .
N6 C1 K1 123.98(8) . .
N2 C1 K1 119.76(8) . .
N2 C3 C4 109.62(12) . .
C5 C4 C3 109.48(12) . .
N6 C5 C4 109.57(12) . .
N2 C7 C8 111.99(11) . .
N2 C7 C9 112.03(12) . .
C8 C7 C9 111.58(13) . .
N6 C10 C11 111.87(11) . .
N6 C10 C12 111.44(11) . .
C11 C10 C12 111.43(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 N1 2.7625(12) .
K1 N1 2.8434(13) 2_575
K1 C1 3.0051(13) .
K1 K1 3.7895(7) 2_575
Si1 N1 1.6689(11) 2_575
Si1 C15 1.885(2) .
Si1 C14 1.894(2) .
Si1 C13 1.8957(14) .
Si2 N1 1.6688(12) .
Si2 C18 1.8852(15) .
Si2 C17 1.8924(15) .
Si2 C16 1.8938(14) .
N1 Si1 1.6689(11) 2_575
N1 K1 2.8434(13) 2_575
N2 C1 1.347(2) .
N2 C3 1.469(2) .
N2 C7 1.475(2) .
N6 C1 1.344(2) .
N6 C5 1.472(2) .
N6 C10 1.475(2) .
C3 C4 1.512(2) .
C4 C5 1.507(2) .
C7 C8 1.512(2) .
C7 C9 1.514(2) .
C10 C11 1.524(2) .
C10 C12 1.529(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C18 Si2 N1 Si1 -20.77(12) . 2_575
C17 Si2 N1 Si1 102.24(11) . 2_575
C16 Si2 N1 Si1 -141.25(10) . 2_575
C18 Si2 N1 K1 119.77(6) . .
C17 Si2 N1 K1 -117.21(6) . .
C16 Si2 N1 K1 -0.70(7) . .
C18 Si2 N1 K1 -150.32(6) . 2_575
C17 Si2 N1 K1 -27.31(7) . 2_575
C16 Si2 N1 K1 89.20(7) . 2_575
N1 K1 N1 Si2 106.83(6) 2_575 .
C1 K1 N1 Si2 -85.15(6) . .
K1 K1 N1 Si2 106.83(6) 2_575 .
N1 K1 N1 Si1 -100.83(6) 2_575 2_575
C1 K1 N1 Si1 67.20(6) . 2_575
K1 K1 N1 Si1 -100.83(6) 2_575 2_575
N1 K1 N1 K1 0.0 2_575 2_575
C1 K1 N1 K1 168.03(3) . 2_575
K1 K1 N1 K1 0.0 2_575 2_575
C5 N6 C1 N2 -0.6(2) . .
C10 N6 C1 N2 -178.73(10) . .
C5 N6 C1 K1 -179.92(9) . .
C10 N6 C1 K1 1.97(15) . .
C3 N2 C1 N6 2.7(2) . .
C7 N2 C1 N6 179.59(11) . .
C3 N2 C1 K1 -178.01(10) . .
C7 N2 C1 K1 -1.08(14) . .
N1 K1 C1 N6 19.79(11) . .
N1 K1 C1 N6 177.54(8) 2_575 .
K1 K1 C1 N6 49.1(2) 2_575 .
N1 K1 C1 N2 -159.49(8) . .
N1 K1 C1 N2 -1.74(13) 2_575 .
K1 K1 C1 N2 -130.16(9) 2_575 .
C1 N2 C3 C4 24.3(2) . .
C7 N2 C3 C4 -152.68(12) . .
N2 C3 C4 C5 -51.0(2) . .
C1 N6 C5 C4 -28.1(2) . .
C10 N6 C5 C4 150.01(12) . .
C3 C4 C5 N6 52.8(2) . .
C1 N2 C7 C8 -102.23(15) . .
C3 N2 C7 C8 75.0(2) . .
C1 N2 C7 C9 131.52(13) . .
C3 N2 C7 C9 -51.3(2) . .
C1 N6 C10 C11 -128.28(13) . .
C5 N6 C10 C11 53.5(2) . .
C1 N6 C10 C12 106.23(13) . .
C5 N6 C10 C12 -72.04(15) . .
