#------------------------------------------------------------------------------
#$Date: 2025-08-22 00:24:23 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301857 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114467.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_7114467
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_formula_structural     '[K(thf)2(Me3SiNCPhCHCPhNSiMe3)]n'
_chemical_formula_sum            'C29 H45 K N2 O2 Si2'
_chemical_formula_weight         548.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.05(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.217(3)
_cell_length_b                   19.020(3)
_cell_length_c                   15.526(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      14
_cell_volume                     3307.7(12)
_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      253(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           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6061
_diffrn_reflns_theta_max         65.95
_diffrn_reflns_theta_min         3.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_obs          0.0693
_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)+(0.0815P)²+2.8932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2055
_refine_ls_wR_factor_obs         0.1674
_reflns_number_observed          3500
_reflns_number_total             5756
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205296b.txt
_cod_data_source_block           mfl-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.8932P] 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^)+(0.0815P)^2^+2.8932P] 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)/n
_cod_database_code               7114467
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
K K 0.20210(9) 0.27194(6) 0.95067(6) 0.0642(3) Uani 1 d .
Si1 Si 0.15975(13) 0.40806(6) 0.75777(8) 0.0631(4) Uani 1 d .
Si2 Si -0.30406(13) 0.38016(7) 0.62540(8) 0.0635(4) Uani 1 d .
O1 O 0.4153(4) 0.2199(3) 0.8986(3) 0.1058(14) Uani 1 d .
O2 O -0.0057(4) 0.3295(3) 1.0029(3) 0.133(2) Uani 1 d .
N1 N 0.1215(3) 0.3248(2) 0.7877(2) 0.0528(9) Uani 1 d .
N2 N -0.2463(3) 0.2980(2) 0.6094(2) 0.0535(9) Uani 1 d .
C1 C 0.0352(4) 0.2850(2) 0.7528(2) 0.0454(9) Uani 1 d .
C2 C -0.0589(4) 0.3079(2) 0.6962(2) 0.0490(10) Uani 1 d .
H2 H -0.0642(4) 0.3565(2) 0.6909(2) 0.059 Uiso 1 calc R
C3 C -0.1478(4) 0.2707(2) 0.6454(2) 0.0452(9) Uani 1 d .
C4 C 0.0389(4) 0.2101(2) 0.7833(2) 0.0469(10) Uani 1 d .
C5 C -0.0581(4) 0.1761(2) 0.8136(3) 0.0608(12) Uani 1 d .
H5 H -0.1310(4) 0.1993(2) 0.8157(3) 0.073 Uiso 1 calc R
C6 C -0.0467(6) 0.1056(3) 0.8418(4) 0.089(2) Uani 1 d .
H6 H -0.1130(6) 0.0822(3) 0.8611(4) 0.107 Uiso 1 calc R
C7 C 0.0593(7) 0.0720(3) 0.8411(4) 0.098(2) Uani 1 d .
H7 H 0.0657(7) 0.0256(3) 0.8600(4) 0.117 Uiso 1 calc R
C8 C 0.1554(6) 0.1052(3) 0.8132(4) 0.088(2) Uani 1 d .
H8 H 0.2281(6) 0.0818(3) 0.8129(4) 0.105 Uiso 1 calc R
C9 C 0.1472(4) 0.1739(2) 0.7848(3) 0.0613(12) Uani 1 d .
H9 H 0.2149(4) 0.1963(2) 0.7663(3) 0.074 Uiso 1 calc R
C10 C -0.1297(4) 0.1941(2) 0.6246(2) 0.0446(9) Uani 1 d .
C11 C -0.2245(4) 0.1477(2) 0.6299(3) 0.0577(11) Uani 1 d .
H11 H -0.2975(4) 0.1642(2) 0.6472(3) 0.069 Uiso 1 calc R
C12 C -0.2122(5) 0.0768(2) 0.6099(3) 0.0749(14) Uani 1 d .
H12 H -0.2763(5) 0.0463(2) 0.6144(3) 0.090 Uiso 1 calc R
C13 C -0.1062(6) 0.0522(3) 0.5837(3) 0.080(2) Uani 1 d .
H13 H -0.0975(6) 0.0049(3) 0.5706(3) 0.096 Uiso 1 calc R
C14 C -0.0130(5) 0.0971(3) 0.5766(3) 0.078(2) Uani 1 d .
H14 H 0.0593(5) 0.0802(3) 0.5584(3) 0.093 Uiso 1 calc R
C15 C -0.0244(4) 0.1680(2) 0.5962(3) 0.0578(11) Uani 1 d .
H15 H 0.0399(4) 0.1981(2) 0.5900(3) 0.069 Uiso 1 calc R
C16 C 0.2986(6) 0.4307(3) 0.8227(4) 0.110(2) Uani 1 d .
H16A H 0.2837(6) 0.4283(3) 0.8829(4) 0.165 Uiso 1 calc R
H16B H 0.3232(6) 0.4774(3) 0.8086(4) 0.165 Uiso 1 calc R
H16C H 0.3605(6) 0.3980(3) 0.8100(4) 0.165 Uiso 1 calc R
C17 C 0.0487(6) 0.4779(3) 0.7810(5) 0.114(2) Uani 1 d .
H17A H -0.0250(6) 0.4686(3) 0.7489(5) 0.172 Uiso 1 calc R
H17B H 0.0790(6) 0.5229(3) 0.7646(5) 0.172 Uiso 1 calc R
H17C H 0.0352(6) 0.4781(3) 0.8416(5) 0.172 Uiso 1 calc R
C18 C 0.1888(6) 0.4128(3) 0.6409(3) 0.099(2) Uani 1 d .
H18A H 0.1173(6) 0.4011(3) 0.6073(3) 0.148 Uiso 1 calc R
H18B H 0.2508(6) 0.3801(3) 0.6283(3) 0.148 Uiso 1 calc R
H18C H 0.2135(6) 0.4595(3) 0.6268(3) 0.148 Uiso 1 calc R
C19 C -0.3105(5) 0.4064(3) 0.7406(3) 0.084(2) Uani 1 d .
H19A H -0.3511(5) 0.3707(3) 0.7714(3) 0.126 Uiso 1 calc R
H19B H -0.3528(5) 0.4501(3) 0.7442(3) 0.126 Uiso 1 calc R
H19C H -0.2309(5) 0.4120(3) 0.7655(3) 0.126 Uiso 1 calc R
C20 C -0.2253(6) 0.4496(3) 0.5662(4) 0.096(2) Uani 1 d .
H20A H -0.2218(6) 0.4363(3) 0.5068(4) 0.144 Uiso 1 calc R
H20B H -0.1458(6) 0.4551(3) 0.5913(4) 0.144 Uiso 1 calc R
H20C H -0.2677(6) 0.4932(3) 0.5700(4) 0.144 Uiso 1 calc R
C21 C -0.4615(6) 0.3760(3) 0.5806(5) 0.116(2) Uani 1 d .
H21A H -0.5038(6) 0.3404(3) 0.6103(5) 0.174 Uiso 1 calc R
H21B H -0.4623(6) 0.3648(3) 0.5202(5) 0.174 Uiso 1 calc R
H21C H -0.4993(6) 0.4207(3) 0.5880(5) 0.174 Uiso 1 calc R
C22 C 0.4772(8) 0.2461(6) 0.8322(6) 0.183(5) Uani 1 d .
H22A H 0.4975(8) 0.2950(6) 0.8430(6) 0.219 Uiso 1 calc R
H22B H 0.4289(8) 0.2433(6) 0.7786(6) 0.219 Uiso 1 calc R
C23 C 0.5823(9) 0.2057(8) 0.8263(7) 0.215(6) Uani 1 d .
H23A H 0.5769(9) 0.1770(8) 0.7746(7) 0.258 Uiso 1 calc R
H23B H 0.6511(9) 0.2364(8) 0.8235(7) 0.258 Uiso 1 calc R
C24 C 0.5946(9) 0.1625(6) 0.9001(8) 0.189(5) Uani 1 d .
H24A H 0.6592(9) 0.1790(6) 0.9389(8) 0.227 Uiso 1 calc R
H24B H 0.6107(9) 0.1143(6) 0.8840(8) 0.227 Uiso 1 calc R
C25 C 0.4836(7) 0.1674(5) 0.9395(5) 0.135(3) Uani 1 d .
H25A H 0.4418(7) 0.1228(5) 0.9347(5) 0.162 Uiso 1 calc R
H25B H 0.4969(7) 0.1785(5) 1.0002(5) 0.162 Uiso 1 calc R
C26 C -0.0926(10) 0.3555(8) 0.9498(7) 0.263(8) Uani 1 d .
H26A H -0.0642(10) 0.3981(8) 0.9234(7) 0.316 Uiso 1 calc R
H26B H -0.1108(10) 0.3217(8) 0.9041(7) 0.316 Uiso 1 calc R
C27 C -0.1914(10) 0.3698(9) 0.9888(7) 0.267(9) Uani 1 d .
H27A H -0.2607(10) 0.3509(9) 0.9567(7) 0.321 Uiso 1 calc R
H27B H -0.2014(10) 0.4202(9) 0.9953(7) 0.321 Uiso 1 calc R
C28 C -0.1751(9) 0.3372(10) 1.0691(8) 0.258(8) Uani 1 d .
H28A H -0.2044(9) 0.3666(10) 1.1144(8) 0.310 Uiso 1 calc R
H28B H -0.2159(9) 0.2922(10) 1.0695(8) 0.310 Uiso 1 calc R
C29 C -0.0539(9) 0.3285(8) 1.0794(6) 0.244(8) Uani 1 d .
H29A H -0.0198(9) 0.3659(8) 1.1153(6) 0.293 Uiso 1 calc R
H29B H -0.0362(9) 0.2840(8) 1.1079(6) 0.293 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 K O1 177.5(2) . .
O2 K N1 83.43(13) . .
O1 K N1 96.13(12) . .
O2 K N2 93.91(13) . 2
O1 K N2 86.91(12) . 2
N1 K N2 170.65(11) . 2
O2 K C9 109.8(2) . .
O1 K C9 71.82(13) . .
N1 K C9 56.67(10) . .
N2 K C9 116.51(11) 2 .
O2 K C11 74.86(14) . 2
O1 K C11 103.70(13) . 2
N1 K C11 130.92(11) . 2
N2 K C11 56.22(11) 2 2
C9 K C11 172.18(11) . 2
O2 K C10 98.03(14) . 2
O1 K C10 80.86(12) . 2
N1 K C10 144.18(10) . 2
N2 K C10 45.02(10) 2 2
C9 K C10 148.51(11) . 2
C11 K C10 24.60(10) 2 2
O2 K C4 86.02(14) . .
O1 K C4 95.41(12) . .
N1 K C4 44.55(9) . .
N2 K C4 126.46(10) 2 .
C9 K C4 24.62(10) . .
C11 K C4 160.88(11) 2 .
C10 K C4 170.56(10) 2 .
O2 K C3 102.50(13) . 2
O1 K C3 77.49(11) . 2
N1 K C3 168.09(10) . 2
N2 K C3 21.08(9) 2 2
C9 K C3 128.66(11) . 2
C11 K C3 43.51(10) 2 2
C10 K C3 25.59(9) 2 2
C4 K C3 145.14(10) . 2
O2 K C1 78.94(13) . .
O1 K C1 101.50(11) . .
N1 K C1 20.55(9) . .
N2 K C1 150.11(10) 2 .
C9 K C1 43.21(10) . .
C11 K C1 144.54(10) 2 .
C10 K C1 164.13(10) 2 .
C4 K C1 25.16(9) . .
C3 K C1 170.27(9) 2 .
N1 Si1 C16 106.4(2) . .
N1 Si1 C18 111.6(2) . .
C16 Si1 C18 109.4(3) . .
N1 Si1 C17 115.2(3) . .
C16 Si1 C17 106.1(3) . .
C18 Si1 C17 107.9(3) . .
N2 Si2 C20 112.5(2) . .
N2 Si2 C19 114.7(2) . .
C20 Si2 C19 109.2(3) . .
N2 Si2 C21 105.4(2) . .
C20 Si2 C21 108.1(3) . .
C19 Si2 C21 106.6(3) . .
C22 O1 C25 108.4(6) . .
C22 O1 K 125.1(5) . .
C25 O1 K 126.2(4) . .
C29 O2 C26 103.7(6) . .
C29 O2 K 130.6(5) . .
C26 O2 K 124.8(5) . .
C1 N1 Si1 127.4(3) . .
C1 N1 K 110.8(2) . .
Si1 N1 K 120.0(2) . .
C3 N2 Si2 127.7(3) . .
C3 N2 K 108.2(2) . 2_454
Si2 N2 K 119.5(2) . 2_454
N1 C1 C2 126.0(4) . .
N1 C1 C4 114.0(4) . .
C2 C1 C4 119.9(4) . .
N1 C1 K 48.6(2) . .
C2 C1 K 156.1(3) . .
C4 C1 K 69.7(2) . .
C1 C2 C3 132.2(4) . .
N2 C3 C2 125.9(4) . .
N2 C3 C10 114.1(3) . .
C2 C3 C10 119.9(4) . .
N2 C3 K 50.7(2) . 2_454
C2 C3 K 152.7(3) . 2_454
C10 C3 K 69.7(2) . 2_454
C5 C4 C9 118.0(4) . .
C5 C4 C1 123.1(4) . .
C9 C4 C1 118.9(4) . .
C5 C4 K 108.3(3) . .
C9 C4 K 73.7(2) . .
C1 C4 K 85.1(2) . .
C4 C5 C6 119.5(5) . .
C7 C6 C5 120.8(5) . .
C8 C7 C6 120.1(5) . .
C7 C8 C9 120.6(6) . .
C8 C9 C4 121.0(5) . .
C8 C9 K 106.7(3) . .
C4 C9 K 81.7(2) . .
C15 C10 C11 117.5(4) . .
C15 C10 C3 123.1(4) . .
C11 C10 C3 119.3(4) . .
C15 C10 K 105.9(3) . 2_454
C11 C10 K 76.4(2) . 2_454
C3 C10 K 84.7(2) . 2_454
C10 C11 C12 121.2(4) . .
C10 C11 K 79.0(2) . 2_454
C12 C11 K 106.7(3) . 2_454
C13 C12 C11 119.9(5) . .
C14 C13 C12 119.8(5) . .
C13 C14 C15 120.8(5) . .
C10 C15 C14 120.8(4) . .
O1 C22 C23 108.0(8) . .
C24 C23 C22 108.0(7) . .
C23 C24 C25 105.2(8) . .
O1 C25 C24 109.0(7) . .
C27 C26 O2 113.4(8) . .
C26 C27 C28 104.1(9) . .
C29 C28 C27 103.9(9) . .
O2 C29 C28 110.0(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K O2 2.737(4) .
K O1 2.749(4) .
K N1 2.827(3) .
K N2 2.833(3) 2
K C9 3.213(5) .
K C11 3.243(5) 2
K C10 3.275(4) 2
K C4 3.314(4) .
K C3 3.478(4) 2
K C1 3.520(4) .
Si1 N1 1.711(3) .
Si1 C16 1.860(6) .
Si1 C18 1.863(5) .
Si1 C17 1.869(6) .
Si2 N2 1.715(3) .
Si2 C20 1.859(6) .
Si2 C19 1.862(5) .
Si2 C21 1.865(6) .
O1 C22 1.367(8) .
O1 C25 1.391(8) .
O2 C29 1.331(9) .
O2 C26 1.336(9) .
N1 C1 1.322(5) .
N2 C3 1.317(5) .
N2 K 2.833(3) 2_454
C1 C2 1.406(5) .
C1 C4 1.502(5) .
C2 C3 1.426(5) .
C3 C10 1.509(5) .
C3 K 3.478(4) 2_454
C4 C5 1.371(6) .
C4 C9 1.395(6) .
C5 C6 1.415(7) .
C6 C7 1.352(8) .
C7 C8 1.341(8) .
C8 C9 1.379(6) .
C10 C15 1.375(6) .
C10 C11 1.389(6) .
C10 K 3.275(4) 2_454
C11 C12 1.392(6) .
C11 K 3.243(5) 2_454
C12 C13 1.359(7) .
C13 C14 1.359(7) .
C14 C15 1.389(6) .
C22 C23 1.414(11) .
C23 C24 1.410(11) .
C24 C25 1.419(10) .
C26 C27 1.319(10) .
C27 C28 1.396(13) .
C28 C29 1.370(12) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139184974
