#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:46:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179423 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/20/4332042.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_4332042
loop_
_publ_author_name
'Evans, William J.'
'Rego, Daniel B.'
'Ziller, Joseph W.'
_publ_section_title
;
 Lanthanum and Alkali Metal Coordination Chemistry of the
 Bis(dimethylphenylsilyl)amide Ligand
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3437
_journal_page_last               3443
_journal_paper_doi               10.1021/ic052091c
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C46 H60 K2 N2 Si4'
_chemical_formula_weight         831.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.917(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.300(5)
_cell_length_b                   13.331(4)
_cell_length_c                   20.992(6)
_cell_measurement_temperature    163(2)
_cell_volume                     4751(2)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24674
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.8649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+3.1721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                4674
_reflns_number_total             5748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052091csup1.cif
_cod_data_source_block           dbr9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4332042
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'
'-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
K1 K 0.019013(17) 0.35684(2) 0.010692(16) 0.02174(8) Uani 1 1 d
Si1 Si 0.13516(2) 0.54725(3) 0.126268(19) 0.01888(9) Uani 1 1 d
Si2 Si 0.17439(2) 0.53857(3) -0.00289(2) 0.01910(9) Uani 1 1 d
N1 N 0.11961(6) 0.52039(8) 0.04446(6) 0.0194(2) Uani 1 1 d
C1 C 0.12143(8) 0.68702(10) 0.13758(7) 0.0199(3) Uani 1 1 d
C2 C 0.17621(9) 0.75546(11) 0.13047(8) 0.0270(3) Uani 1 1 d
C3 C 0.16912(10) 0.85828(12) 0.13693(9) 0.0314(3) Uani 1 1 d
C4 C 0.10610(9) 0.89636(11) 0.15049(8) 0.0289(3) Uani 1 1 d
C5 C 0.05039(9) 0.83133(12) 0.15703(8) 0.0283(3) Uani 1 1 d
C6 C 0.05817(8) 0.72809(11) 0.15066(7) 0.0232(3) Uani 1 1 d
C7 C 0.06007(10) 0.48105(12) 0.15278(9) 0.0273(3) Uani 1 1 d
C8 C 0.23358(10) 0.51215(14) 0.19234(9) 0.0324(4) Uani 1 1 d
C9 C 0.15991(7) 0.42962(10) -0.06478(7) 0.0196(3) Uani 1 1 d
C10 C 0.16539(8) 0.33156(10) -0.03998(7) 0.0203(3) Uani 1 1 d
C11 C 0.15767(8) 0.24833(11) -0.08219(8) 0.0242(3) Uani 1 1 d
C12 C 0.14454(8) 0.26155(12) -0.15098(8) 0.0269(3) Uani 1 1 d
C13 C 0.13896(9) 0.35794(13) -0.17704(8) 0.0288(3) Uani 1 1 d
C14 C 0.14658(9) 0.44048(12) -0.13456(8) 0.0254(3) Uani 1 1 d
C15 C 0.28437(9) 0.54680(13) 0.04483(10) 0.0298(3) Uani 1 1 d
C16 C 0.14820(10) 0.65542(12) -0.05747(9) 0.0297(3) Uani 1 1 d
C17 C 0.08810(10) 0.18955(12) 0.16639(9) 0.0312(3) Uani 1 1 d
C18 C 0.01404(10) 0.16151(13) 0.12021(10) 0.0350(4) Uani 1 1 d
C19 C 0.00334(10) 0.12740(12) 0.05511(10) 0.0355(4) Uani 1 1 d
C20 C 0.06715(10) 0.12006(12) 0.03479(9) 0.0324(4) Uani 1 1 d
C21 C 0.14144(9) 0.14792(12) 0.08044(9) 0.0302(3) Uani 1 1 d
C22 C 0.15130(9) 0.18281(12) 0.14503(9) 0.0297(3) Uani 1 1 d
C23 C 0.10075(15) 0.2247(2) 0.23798(11) 0.0488(5) Uani 1 1 d
H2 H 0.2198(10) 0.7343(14) 0.1197(9) 0.030(4) Uiso 1 1 d
H3 H 0.2089(11) 0.9064(15) 0.1325(10) 0.041(5) Uiso 1 1 d
H4 H 0.1011(10) 0.9641(14) 0.1553(9) 0.028(4) Uiso 1 1 d
H5 H 0.0047(11) 0.8556(14) 0.1658(10) 0.036(5) Uiso 1 1 d
H6 H 0.0201(10) 0.6868(14) 0.1572(9) 0.031(5) Uiso 1 1 d
H7A H 0.0624(11) 0.4958(15) 0.1976(10) 0.038(5) Uiso 1 1 d
H7B H 0.0694(11) 0.4107(17) 0.1552(10) 0.042(5) Uiso 1 1 d
H7C H 0.0064(12) 0.4930(15) 0.1227(10) 0.038(5) Uiso 1 1 d
H8A H 0.2756(13) 0.5500(17) 0.1856(11) 0.054(6) Uiso 1 1 d
H8B H 0.2348(12) 0.5281(16) 0.2390(11) 0.047(6) Uiso 1 1 d
H8C H 0.2413(13) 0.440(2) 0.1879(12) 0.063(7) Uiso 1 1 d
H10 H 0.1758(9) 0.3203(12) 0.0078(8) 0.019(4) Uiso 1 1 d
H11 H 0.1611(10) 0.1836(15) -0.0642(9) 0.034(5) Uiso 1 1 d
H12 H 0.1387(10) 0.2070(14) -0.1810(9) 0.030(4) Uiso 1 1 d
H12 H 0.1303(10) 0.3669(13) -0.2242(10) 0.033(5) Uiso 1 1 d
H14 H 0.1414(11) 0.5065(15) -0.1542(10) 0.038(5) Uiso 1 1 d
H15A H 0.3108(13) 0.5491(16) 0.0142(11) 0.051(6) Uiso 1 1 d
H15B H 0.3043(11) 0.4905(15) 0.0762(10) 0.037(5) Uiso 1 1 d
H15C H 0.2993(12) 0.6068(17) 0.0752(10) 0.049(6) Uiso 1 1 d
H16A H 0.1509(11) 0.7129(16) -0.0286(10) 0.040(5) Uiso 1 1 d
H16B H 0.0927(12) 0.6553(15) -0.0937(10) 0.043(5) Uiso 1 1 d
H16C H 0.1835(12) 0.6657(16) -0.0812(10) 0.047(6) Uiso 1 1 d
H18 H -0.0287(12) 0.1657(16) 0.1341(10) 0.049(6) Uiso 1 1 d
H19 H -0.0464(12) 0.1087(16) 0.0241(10) 0.045(5) Uiso 1 1 d
H20 H 0.0605(10) 0.0954(14) -0.0109(9) 0.033(5) Uiso 1 1 d
H21 H 0.1872(11) 0.1433(14) 0.0670(10) 0.040(5) Uiso 1 1 d
H22 H 0.1999(12) 0.2024(15) 0.1749(10) 0.040(5) Uiso 1 1 d
H23A H 0.0611(15) 0.271(2) 0.2380(12) 0.071(7) Uiso 1 1 d
H23B H 0.0944(17) 0.169(2) 0.2643(16) 0.090(9) Uiso 1 1 d
H23C H 0.1510(17) 0.254(2) 0.2604(14) 0.085(9) Uiso 1 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 N1 93.28(4) . 5_565
N1 K1 C19 142.27(4) . .
N1 K1 C19 119.58(4) 5_565 .
N1 K1 C7 57.27(4) . .
N1 K1 C7 86.93(4) 5_565 .
C19 K1 C7 103.42(5) . .
N1 K1 C10 67.34(4) . .
N1 K1 C10 129.72(4) 5_565 .
C19 K1 C10 99.71(4) . .
C7 K1 C10 114.69(4) . .
N1 K1 C1 126.61(4) . 5_565
N1 K1 C1 57.02(4) 5_565 5_565
C19 K1 C1 89.00(4) . 5_565
C7 K1 C1 142.88(4) . 5_565
C10 K1 C1 96.96(4) . 5_565
N1 K1 C20 127.32(4) . .
N1 K1 C20 139.40(4) 5_565 .
C19 K1 C20 24.63(4) . .
C7 K1 C20 113.22(5) . .
C10 K1 C20 75.09(4) . .
C1 K1 C20 92.60(4) 5_565 .
N1 K1 C6 120.99(4) . 5_565
N1 K1 C6 79.00(4) 5_565 5_565
C19 K1 C6 85.56(5) . 5_565
C7 K1 C6 165.78(4) . 5_565
C10 K1 C6 73.81(4) . 5_565
C1 K1 C6 24.38(3) 5_565 5_565
C20 K1 C6 79.46(4) . 5_565
N1 K1 Si1 100.43(3) . 5_565
N1 K1 Si1 29.01(2) 5_565 5_565
C19 K1 Si1 117.30(3) . 5_565
C7 K1 Si1 114.54(4) . 5_565
C10 K1 Si1 106.54(3) . 5_565
C1 K1 Si1 32.94(3) 5_565 5_565
C20 K1 Si1 125.39(3) . 5_565
C6 K1 Si1 51.23(3) 5_565 5_565
N1 K1 C18 126.57(4) . .
N1 K1 C18 116.95(4) 5_565 .
C19 K1 C18 23.29(5) . .
C7 K1 C18 80.19(5) . .
C10 K1 C18 111.41(4) . .
C1 K1 C18 106.79(4) 5_565 .
C20 K1 C18 41.42(4) . .
C6 K1 C18 108.00(5) 5_565 .
Si1 K1 C18 127.77(3) 5_565 .
N1 K1 C21 104.86(4) . .
N1 K1 C21 160.73(4) 5_565 .
C19 K1 C21 41.16(4) . .
C7 K1 C21 97.35(5) . .
C10 K1 C21 65.21(4) . .
C1 K1 C21 113.94(4) 5_565 .
C20 K1 C21 23.18(4) . .
C6 K1 C21 96.64(4) 5_565 .
Si1 K1 C21 146.73(3) 5_565 .
C18 K1 C21 46.24(4) . .
N1 K1 Si1 26.48(3) . .
N1 K1 Si1 94.60(3) 5_565 .
C19 K1 Si1 124.33(4) . .
C7 K1 Si1 31.36(3) . .
C10 K1 Si1 86.69(3) . .
C1 K1 Si1 145.50(3) 5_565 .
C20 K1 Si1 121.28(4) . .
C6 K1 Si1 147.16(3) 5_565 .
Si1 K1 Si1 113.256(19) 5_565 .
C18 K1 Si1 103.61(4) . .
C21 K1 Si1 98.79(3) . .
N1 Si1 C8 117.02(7) . .
N1 Si1 C7 109.88(7) . .
C8 Si1 C7 105.64(9) . .
N1 Si1 C1 110.94(6) . .
C8 Si1 C1 106.64(7) . .
C7 Si1 C1 106.05(7) . .
N1 Si1 K1 56.51(4) . 5_565
C8 Si1 K1 166.66(6) . 5_565
C7 Si1 K1 87.70(6) . 5_565
C1 Si1 K1 68.61(4) . 5_565
N1 Si1 K1 47.64(4) . .
C8 Si1 K1 118.94(6) . .
C7 Si1 K1 63.71(5) . .
C1 Si1 K1 134.41(4) . .
K1 Si1 K1 66.744(19) 5_565 .
N1 Si2 C16 114.09(7) . .
N1 Si2 C15 116.76(8) . .
C16 Si2 C15 104.66(8) . .
N1 Si2 C9 109.52(6) . .
C16 Si2 C9 106.07(7) . .
C15 Si2 C9 104.84(7) . .
N1 Si2 K1 46.72(4) . 5_565
C16 Si2 K1 69.20(5) . 5_565
C15 Si2 K1 143.49(6) . 5_565
C9 Si2 K1 111.46(4) . 5_565
N1 Si2 K1 40.25(4) . .
C16 Si2 K1 122.73(6) . .
C15 Si2 K1 132.24(6) . .
C9 Si2 K1 69.46(4) . .
K1 Si2 K1 61.52(2) 5_565 .
Si1 N1 Si2 132.06(7) . .
Si1 N1 K1 105.87(5) . .
Si2 N1 K1 116.79(6) . .
Si1 N1 K1 94.48(5) . 5_565
Si2 N1 K1 108.23(6) . 5_565
K1 N1 K1 86.72(4) . 5_565
C6 C1 C2 116.29(13) . .
C6 C1 Si1 124.38(11) . .
C2 C1 Si1 119.29(11) . .
C6 C1 K1 80.94(8) . 5_565
C2 C1 K1 110.74(9) . 5_565
Si1 C1 K1 78.45(4) . 5_565
C3 C2 C1 122.33(15) . .
C4 C3 C2 119.86(15) . .
C5 C4 C3 119.49(14) . .
C4 C5 C6 120.22(15) . .
C5 C6 C1 121.80(14) . .
C5 C6 K1 114.30(10) . 5_565
C1 C6 K1 74.68(8) . 5_565
Si1 C7 K1 84.93(6) . .
C10 C9 C14 116.56(13) . .
C10 C9 Si2 119.22(11) . .
C14 C9 Si2 124.18(11) . .
C11 C10 C9 122.13(13) . .
C11 C10 K1 112.99(9) . .
C9 C10 K1 94.11(8) . .
C12 C11 C10 119.93(14) . .
C11 C12 C13 119.26(14) . .
C12 C13 C14 120.39(14) . .
C13 C14 C9 121.73(14) . .
C22 C17 C18 117.97(16) . .
C22 C17 C23 120.32(17) . .
C18 C17 C23 121.70(16) . .
C19 C18 C17 121.25(16) . .
C19 C18 K1 67.92(9) . .
C17 C18 K1 90.02(10) . .
C18 C19 C20 120.11(16) . .
C18 C19 K1 88.79(10) . .
C20 C19 K1 78.65(9) . .
C19 C20 C21 119.20(17) . .
C19 C20 K1 76.72(9) . .
C21 C20 K1 89.22(10) . .
C22 C21 C20 120.19(15) . .
C22 C21 K1 88.37(10) . .
C20 C21 K1 67.60(9) . .
C21 C22 C17 121.27(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 N1 2.7697(13) .
K1 N1 2.8744(13) 5_565
K1 C19 3.2414(18) .
K1 C7 3.2450(18) .
K1 C10 3.2477(16) .
K1 C1 3.2654(15) 5_565
K1 C20 3.2654(18) .
K1 C6 3.3434(16) 5_565
K1 Si1 3.4359(8) 5_565
K1 C18 3.4971(18) .
K1 C21 3.5315(17) .
K1 Si1 3.6052(8) .
Si1 N1 1.6714(13) .
Si1 C8 1.8767(16) .
Si1 C7 1.8835(16) .
Si1 C1 1.9068(15) .
Si1 K1 3.4359(8) 5_565
Si2 N1 1.6718(13) .
Si2 C16 1.8866(17) .
Si2 C15 1.8872(16) .
Si2 C9 1.9002(15) .
Si2 K1 3.7502(10) 5_565
N1 K1 2.8744(13) 5_565
C1 C6 1.397(2) .
C1 C2 1.404(2) .
C1 K1 3.2654(15) 5_565
C2 C3 1.388(2) .
C3 C4 1.384(2) .
C4 C5 1.383(2) .
C5 C6 1.395(2) .
C6 K1 3.3434(16) 5_565
C9 C10 1.397(2) .
C9 C14 1.400(2) .
C10 C11 1.394(2) .
C11 C12 1.384(2) .
C12 C13 1.385(2) .
C13 C14 1.390(2) .
C17 C22 1.391(2) .
C17 C18 1.391(3) .
C17 C23 1.507(3) .
C18 C19 1.383(3) .
C19 C20 1.388(3) .
C20 C21 1.390(2) .
C21 C22 1.380(2) .
