#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:21:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114470.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7114470
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Liu, Diang-Sheng'
'Sablong, Rafaël'
_publ_section_title
;
 Syntheses and structures of structurally diverse potassium
 β-diketiminates derived from the ligand
 [{N(SiMe₃)C(Ph)}₂CH]⁻
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1920
_journal_page_last               1921
_journal_paper_doi               10.1039/b205296b
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H82 K2 N4 O6 Si2'
_chemical_formula_structural     'C58 H82 K2 N4 O6 Si2'
_chemical_formula_sum            'C58 H82 K2 N4 O6 Si2'
_chemical_formula_weight         1065.66
_chemical_name_common            '[{K(thf)3(C3HPh2N2SiMe2)}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             2000-01-31T16:23:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.978(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5035(4)
_cell_length_b                   18.0757(7)
_cell_length_c                   14.5585(6)
_cell_measurement_reflns_used    13337
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     2971.8(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1145
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29045
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         4.57
_exptl_absorpt_coefficient_mu    0.25
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.9517
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0775
_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)+(0.0830P)²+6.2106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.177
_refine_ls_wR_factor_ref         0.2051
_reflns_number_gt                3421
_reflns_number_total             5226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205296b.txt
_cod_data_source_block           mfl-4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114470
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 0.03412(9) 0.07793(5) 0.82153(7) 0.0391(3) Uani 1 1 d .
Si Si 0.02811(9) 0.11774(6) 1.08072(8) 0.0300(3) Uani 1 1 d .
O1 O -0.0837(3) 0.20845(19) 0.8209(3) 0.0604(10) Uani 1 1 d .
O2 O 0.1900(3) -0.0121(2) 0.7556(3) 0.0641(11) Uani 1 1 d .
O3 O 0.0850(10) 0.1629(6) 0.6721(5) 0.241(6) Uani 1 1 d .
N1 N 0.1270(3) 0.12478(18) 1.0050(2) 0.0309(8) Uani 1 1 d .
N2 N 0.0858(3) 0.05649(19) 1.1691(2) 0.0323(8) Uani 1 1 d .
C1 C 0.2393(3) 0.1109(2) 1.0422(3) 0.0293(9) Uani 1 1 d .
C2 C 0.2802(3) 0.0802(2) 1.1314(3) 0.0322(9) Uani 1 1 d .
H2 H 0.363 0.0796 1.1554 0.039 Uiso 1 1 calc R
C3 C 0.2032(3) 0.0502(2) 1.1868(3) 0.0290(9) Uani 1 1 d .
C4 C 0.3292(3) 0.1270(2) 0.9813(3) 0.0318(9) Uani 1 1 d .
C5 C 0.3005(4) 0.1761(3) 0.9065(3) 0.0432(11) Uani 1 1 d .
H5 H 0.2251 0.1994 0.8953 0.052 Uiso 1 1 calc R
C6 C 0.3796(4) 0.1915(3) 0.8484(4) 0.0516(13) Uani 1 1 d .
H6 H 0.3579 0.2248 0.7975 0.062 Uiso 1 1 calc R
C7 C 0.4896(4) 0.1588(3) 0.8640(4) 0.0487(13) Uani 1 1 d .
H7 H 0.5439 0.1695 0.8241 0.058 Uiso 1 1 calc R
C8 C 0.5204(4) 0.1108(3) 0.9376(3) 0.0452(12) Uani 1 1 d .
H8 H 0.5965 0.0883 0.9489 0.054 Uiso 1 1 calc R
C9 C 0.4409(3) 0.0947(2) 0.9957(3) 0.0365(10) Uani 1 1 d .
H9 H 0.4633 0.0611 1.0461 0.044 Uiso 1 1 calc R
C10 C 0.2571(3) 0.0056(2) 1.2717(3) 0.0313(9) Uani 1 1 d .
C11 C 0.1999(4) 0.0009(3) 1.3465(3) 0.0435(11) Uani 1 1 d .
H11 H 0.1253 0.0244 1.3427 0.052 Uiso 1 1 calc R
C12 C 0.2486(5) -0.0372(3) 1.4270(4) 0.0596(15) Uani 1 1 d .
H12 H 0.2088 -0.0383 1.4785 0.072 Uiso 1 1 calc R
C13 C 0.3558(5) -0.0740(3) 1.4326(4) 0.0621(15) Uani 1 1 d .
H13 H 0.3893 -0.1007 1.4875 0.075 Uiso 1 1 calc R
C14 C 0.4128(4) -0.0712(3) 1.3578(4) 0.0525(13) Uani 1 1 d .
H14 H 0.4861 -0.0963 1.3611 0.063 Uiso 1 1 calc R
C15 C 0.3648(4) -0.0322(2) 1.2781(3) 0.0402(11) Uani 1 1 d .
H15 H 0.4051 -0.0311 1.2269 0.048 Uiso 1 1 calc R
C16 C 0.0039(4) 0.2107(3) 1.1316(3) 0.0428(11) Uani 1 1 d .
H16A H -0.0523 0.2058 1.174 0.064 Uiso 1 1 calc R
H16B H -0.028 0.2451 1.081 0.064 Uiso 1 1 calc R
H16C H 0.0794 0.2297 1.1662 0.064 Uiso 1 1 calc R
C17 C -0.1201(4) 0.0867(3) 1.0179(3) 0.0384(10) Uani 1 1 d .
H17A H -0.1743 0.0834 1.0622 0.058 Uiso 1 1 calc R
H17B H -0.113 0.038 0.99 0.058 Uiso 1 1 calc R
H17C H -0.1511 0.1223 0.9686 0.058 Uiso 1 1 calc R
C18 C -0.0265(4) 0.2720(3) 0.8684(4) 0.0588(14) Uani 1 1 d .
H18A H 0.0207 0.298 0.8281 0.071 Uiso 1 1 calc R
H18B H 0.0273 0.2569 0.9268 0.071 Uiso 1 1 calc R
C19 C -0.1223(5) 0.3219(3) 0.8902(5) 0.0649(16) Uani 1 1 d .
H19A H -0.1164 0.3718 0.8635 0.078 Uiso 1 1 calc R
H19B H -0.117 0.3265 0.9587 0.078 Uiso 1 1 calc R
C20 C -0.2366(5) 0.2846(3) 0.8453(4) 0.0626(15) Uani 1 1 d .
H20A H -0.2725 0.2583 0.8926 0.075 Uiso 1 1 calc R
H20B H -0.2942 0.3211 0.8127 0.075 Uiso 1 1 calc R
C21 C -0.2002(5) 0.2315(3) 0.7774(4) 0.0662(16) Uani 1 1 d .
H21A H -0.2549 0.1887 0.7668 0.079 Uiso 1 1 calc R
H21B H -0.1993 0.2559 0.7167 0.079 Uiso 1 1 calc R
C22 C 0.1511(4) -0.0740(3) 0.6970(4) 0.0593(15) Uani 1 1 d .
H22A H 0.1179 -0.0575 0.6325 0.071 Uiso 1 1 calc R
H22B H 0.0896 -0.1021 0.7214 0.071 Uiso 1 1 calc R
C23 C 0.2573(5) -0.1201(4) 0.6982(6) 0.087(2) Uani 1 1 d .
H23A H 0.2587 -0.1621 0.7421 0.104 Uiso 1 1 calc R
H23B H 0.2587 -0.14 0.635 0.104 Uiso 1 1 calc R
C24 C 0.3578(5) -0.0713(4) 0.7289(7) 0.119(4) Uani 1 1 d .
H24A H 0.4242 -0.0986 0.7674 0.143 Uiso 1 1 calc R
H24B H 0.3854 -0.0494 0.6745 0.143 Uiso 1 1 calc R
C25 C 0.3152(5) -0.0146(4) 0.7833(6) 0.085(2) Uani 1 1 d .
H25A H 0.3375 -0.0262 0.8508 0.102 Uiso 1 1 calc R
H25B H 0.3501 0.0338 0.7719 0.102 Uiso 1 1 calc R
C26 C 0.0318(13) 0.2159(7) 0.6251(8) 0.160(5) Uani 1 1 d .
H26A H 0.084 0.259 0.622 0.192 Uiso 1 1 calc R
H26B H -0.0401 0.2316 0.648 0.192 Uiso 1 1 calc R
C27 C 0.0045(15) 0.1755(11) 0.5371(11) 0.231(8) Uani 1 1 d .
H27A H -0.0733 0.1505 0.5302 0.277 Uiso 1 1 calc R
H27B H 0.0036 0.209 0.4832 0.277 Uiso 1 1 calc R
C28 C 0.0958(16) 0.1240(8) 0.5438(11) 0.220(8) Uani 1 1 d .
H28A H 0.124 0.1174 0.4842 0.264 Uiso 1 1 calc R
H28B H 0.0752 0.0755 0.568 0.264 Uiso 1 1 calc R
C29 C 0.1752(9) 0.1647(15) 0.6101(11) 0.325(15) Uani 1 1 d .
H29A H 0.192 0.215 0.5889 0.39 Uiso 1 1 calc R
H29B H 0.2494 0.138 0.6359 0.39 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'
O O 0.0106 0.006 '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_1
_geom_angle_site_symmetry_3
O1 K O2 151.25(12) . .
O1 K N2 120.08(11) . 3_557
O2 K N2 82.14(11) . 3_557
O1 K N1 80.84(11) . .
O2 K N1 110.96(11) . .
N2 K N1 108.41(10) 3_557 .
O1 K O3 72.60(19) . .
O2 K O3 78.81(19) . .
N2 K O3 133.3(3) 3_557 .
N1 K O3 118.2(3) . .
N2 Si N1 108.34(16) . .
N2 Si C17 111.00(19) . .
N1 Si C17 111.13(19) . .
N2 Si C16 110.1(2) . .
N1 Si C16 110.46(19) . .
C17 Si C16 105.8(2) . .
C21 O1 C18 106.6(4) . .
C21 O1 K 132.7(3) . .
C18 O1 K 120.7(3) . .
C25 O2 C22 109.2(4) . .
C25 O2 K 128.2(3) . .
C22 O2 K 121.8(3) . .
C26 O3 C29 88.7(12) . .
C26 O3 K 132.9(7) . .
C29 O3 K 138.3(11) . .
C1 N1 Si 115.6(3) . .
C1 N1 K 119.7(2) . .
Si N1 K 113.93(15) . .
C3 N2 Si 115.5(3) . .
C3 N2 K 114.0(3) . 3_557
Si N2 K 117.79(16) . 3_557
N1 C1 C2 125.5(4) . .
N1 C1 C4 116.4(4) . .
C2 C1 C4 118.1(3) . .
C1 C2 C3 122.8(4) . .
N2 C3 C2 125.4(4) . .
N2 C3 C10 116.7(3) . .
C2 C3 C10 117.9(3) . .
C9 C4 C5 117.3(4) . .
C9 C4 C1 123.1(4) . .
C5 C4 C1 119.6(4) . .
C6 C5 C4 121.4(4) . .
C7 C6 C5 120.2(5) . .
C8 C7 C6 119.6(4) . .
C7 C8 C9 120.4(4) . .
C8 C9 C4 121.1(4) . .
C11 C10 C15 117.8(4) . .
C11 C10 C3 119.8(4) . .
C15 C10 C3 122.5(4) . .
C10 C11 C12 121.5(4) . .
C11 C12 C13 120.1(5) . .
C14 C13 C12 119.2(5) . .
C13 C14 C15 120.6(5) . .
C14 C15 C10 120.8(4) . .
O1 C18 C19 107.1(4) . .
C18 C19 C20 104.7(5) . .
C21 C20 C19 104.1(4) . .
O1 C21 C20 104.5(5) . .
O2 C22 C23 105.8(4) . .
C24 C23 C22 105.5(5) . .
C25 C24 C23 105.5(5) . .
O2 C25 C24 107.5(5) . .
O3 C26 C27 95.6(11) . .
O3 C26 C29 50.6(8) . .
C27 C26 C29 73.0(9) . .
C28 C27 C26 103.9(11) . .
C27 C28 C29 94.7(12) . .
C28 C29 O3 88.2(11) . .
C28 C29 C26 82.6(9) . .
O3 C29 C26 40.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K O1 2.720(3) .
K O2 2.727(3) .
K N2 2.810(4) 3_557
K N1 2.811(4) .
K O3 2.814(7) .
Si N2 1.732(4) .
Si N1 1.733(3) .
Si C17 1.861(4) .
Si C16 1.878(5) .
O1 C21 1.431(6) .
O1 C18 1.435(6) .
O2 C25 1.420(6) .
O2 C22 1.427(6) .
O3 C26 1.265(11) .
O3 C29 1.499(12) .
N1 C1 1.326(5) .
N2 C3 1.330(5) .
N2 K 2.810(4) 3_557
C1 C2 1.408(6) .
C1 C4 1.514(5) .
C2 C3 1.415(6) .
C3 C10 1.506(6) .
C4 C9 1.391(6) .
C4 C5 1.394(6) .
C5 C6 1.384(6) .
C6 C7 1.375(6) .
C7 C8 1.372(7) .
C8 C9 1.389(6) .
C10 C11 1.379(6) .
C10 C15 1.402(6) .
C11 C12 1.382(7) .
C12 C13 1.389(7) .
C13 C14 1.375(7) .
C14 C15 1.380(7) .
C18 C19 1.505(7) .
C19 C20 1.511(7) .
C20 C21 1.494(8) .
C22 C23 1.476(7) .
C23 C24 1.456(8) .
C24 C25 1.436(9) .
C26 C27 1.456(16) .
C26 C29 1.940(19) .
C27 C28 1.393(17) .
C28 C29 1.404(17) .
