#------------------------------------------------------------------------------
#$Date: 2025-08-22 00:24:23 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301857 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114469.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_7114469
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     '[{(Me2NCH2CH2NMe2)K(Me3SiNCPhCHCPhNH)}2]'
_chemical_formula_sum            'C48 H74 K2 N8 Si2'
_chemical_formula_weight         897.53
_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                 94.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.361(3)
_cell_length_b                   16.470(4)
_cell_length_c                   13.088(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2656.2(11)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3420
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    'H on N2 was refined others were riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_obs          0.0604
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0423P)²+2.3196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1431
_refine_ls_wR_factor_obs         0.1194
_reflns_number_observed          2030
_reflns_number_total             3249
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205296b.txt
_cod_data_source_block           mfl-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+2.3196P] 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^)+(0.0423P)^2^+2.3196P] 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               7114469
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 -0.05613(9) 0.11377(7) 0.06934(9) 0.0320(3) Uani 1 d .
Si Si -0.29339(11) 0.03218(9) 0.23267(11) 0.0314(4) Uani 1 d .
N1 N -0.2613(3) 0.0411(2) 0.1091(3) 0.0303(11) Uani 1 d .
N2 N -0.1361(3) -0.0361(3) -0.0418(4) 0.0302(11) Uani 1 d .
H1 H -0.1547(32) -0.0334(25) 0.0154(31) 0.006(13) Uiso 1 d .
N3 N 0.0508(4) 0.2428(3) 0.1788(4) 0.0496(13) Uani 1 d .
N4 N -0.0321(5) 0.2553(3) -0.0418(4) 0.072(2) Uani 1 d .
C1 C -0.3119(4) 0.0752(3) 0.0268(4) 0.0253(12) Uani 1 d .
C2 C -0.2824(4) 0.0639(3) -0.0718(4) 0.0264(12) Uani 1 d .
H2 H -0.3214(4) 0.0937(3) -0.1248(4) 0.032 Uiso 1 calc R
C3 C -0.1979(4) 0.0110(3) -0.1013(4) 0.0256(12) Uani 1 d .
C4 C -0.4048(4) 0.1335(3) 0.0379(4) 0.0284(13) Uani 1 d .
C5 C -0.3861(5) 0.2081(4) 0.0849(4) 0.045(2) Uani 1 d .
H5 H -0.3146(5) 0.2215(4) 0.1115(4) 0.054 Uiso 1 calc R
C6 C -0.4687(5) 0.2632(4) 0.0941(5) 0.056(2) Uani 1 d .
H6 H -0.4537(5) 0.3146(4) 0.1250(5) 0.067 Uiso 1 calc R
C7 C -0.5733(5) 0.2432(4) 0.0581(5) 0.052(2) Uani 1 d .
H7 H -0.6309(5) 0.2805(4) 0.0650(5) 0.063 Uiso 1 calc R
C8 C -0.5937(5) 0.1695(4) 0.0127(4) 0.048(2) Uani 1 d .
H8 H -0.6658(5) 0.1551(4) -0.0110(4) 0.058 Uiso 1 calc R
C9 C -0.5093(4) 0.1159(3) 0.0011(4) 0.0354(13) Uani 1 d .
H9 H -0.5241(4) 0.0657(3) -0.0331(4) 0.042 Uiso 1 calc R
C10 C -0.1794(4) 0.0093(3) -0.2124(4) 0.0258(12) Uani 1 d .
C11 C -0.0740(4) 0.0161(3) -0.2429(4) 0.0343(14) Uani 1 d .
H11 H -0.0145(4) 0.0229(3) -0.1931(4) 0.041 Uiso 1 calc R
C12 C -0.0565(5) 0.0128(3) -0.3458(4) 0.045(2) Uani 1 d .
H12 H 0.0153(5) 0.0172(3) -0.3661(4) 0.053 Uiso 1 calc R
C13 C -0.1409(5) 0.0033(4) -0.4188(4) 0.054(2) Uani 1 d .
H13 H -0.1278(5) 0.0013(4) -0.4892(4) 0.065 Uiso 1 calc R
C14 C -0.2447(5) -0.0033(4) -0.3897(4) 0.051(2) Uani 1 d .
H14 H -0.3036(5) -0.0107(4) -0.4400(4) 0.062 Uiso 1 calc R
C15 C -0.2633(4) 0.0009(3) -0.2873(4) 0.0369(14) Uani 1 d .
H15 H -0.3357(4) -0.0021(3) -0.2681(4) 0.044 Uiso 1 calc R
C16 C -0.4411(4) 0.0342(4) 0.2540(4) 0.0422(15) Uani 1 d .
H16A H -0.4717(4) 0.0870(4) 0.2329(4) 0.063 Uiso 1 calc R
H16B H -0.4504(4) 0.0253(4) 0.3268(4) 0.063 Uiso 1 calc R
H16C H -0.4787(4) -0.0088(4) 0.2133(4) 0.063 Uiso 1 calc R
C17 C -0.2416(4) -0.0702(3) 0.2745(4) 0.0413(15) Uani 1 d .
H17A H -0.1640(4) -0.0740(3) 0.2647(4) 0.062 Uiso 1 calc R
H17B H -0.2810(4) -0.1123(3) 0.2337(4) 0.062 Uiso 1 calc R
H17C H -0.2527(4) -0.0782(3) 0.3472(4) 0.062 Uiso 1 calc R
C18 C -0.2226(4) 0.1110(3) 0.3164(4) 0.049(2) Uani 1 d .
H18A H -0.1449(4) 0.1107(3) 0.3060(4) 0.074 Uiso 1 calc R
H18B H -0.2328(4) 0.0990(3) 0.3883(4) 0.074 Uiso 1 calc R
H18C H -0.2530(4) 0.1646(3) 0.2986(4) 0.074 Uiso 1 calc R
C19 C 0.0590(12) 0.3088(6) 0.1137(8) 0.218(8) Uani 1 d .
H19A H 0.0197(12) 0.3532(6) 0.1459(8) 0.262 Uiso 1 calc R
H19B H 0.1366(12) 0.3242(6) 0.1215(8) 0.262 Uiso 1 calc R
C20 C 0.0311(8) 0.3159(5) 0.0146(6) 0.099(3) Uani 1 d .
H20A H 0.0992(8) 0.3223(5) -0.0197(6) 0.119 Uiso 1 calc R
H20B H -0.0090(8) 0.3678(5) 0.0051(6) 0.119 Uiso 1 calc R
C21 C 0.0008(9) 0.2667(6) 0.2665(8) 0.189(7) Uani 1 d .
H21A H -0.0047(9) 0.2199(6) 0.3121(8) 0.284 Uiso 1 calc R
H21B H -0.0720(9) 0.2877(6) 0.2464(8) 0.284 Uiso 1 calc R
H21C H 0.0443(9) 0.3093(6) 0.3024(8) 0.284 Uiso 1 calc R
C22 C 0.1555(7) 0.2147(5) 0.2088(9) 0.160(5) Uani 1 d .
H22A H 0.1509(7) 0.1681(5) 0.2547(9) 0.240 Uiso 1 calc R
H22B H 0.1973(7) 0.2582(5) 0.2445(9) 0.240 Uiso 1 calc R
H22C H 0.1915(7) 0.1982(5) 0.1480(9) 0.240 Uiso 1 calc R
C23 C -0.1344(9) 0.2865(6) -0.0792(10) 0.203(7) Uani 1 d .
H23A H -0.1759(9) 0.2440(6) -0.1173(10) 0.305 Uiso 1 calc R
H23B H -0.1238(9) 0.3326(6) -0.1247(10) 0.305 Uiso 1 calc R
H23C H -0.1743(9) 0.3045(6) -0.0215(10) 0.305 Uiso 1 calc R
C24 C 0.0245(11) 0.2248(6) -0.1263(7) 0.166(6) Uani 1 d .
H24A H 0.0952(11) 0.2032(6) -0.1003(7) 0.249 Uiso 1 calc R
H24B H 0.0350(11) 0.2690(6) -0.1746(7) 0.249 Uiso 1 calc R
H24C H -0.0184(11) 0.1816(6) -0.1613(7) 0.249 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
N2 K N4 101.1(2) 3 .
N2 K N3 92.39(14) 3 .
N4 K N3 64.5(2) . .
N2 K N1 127.71(13) 3 .
N4 K N1 125.0(2) . .
N3 K N1 126.96(14) . .
N2 K N2 78.93(13) 3 .
N4 K N2 118.9(2) . .
N3 K N2 171.09(14) . .
N1 K N2 59.01(12) . .
N1 Si C16 116.3(2) . .
N1 Si C17 104.9(2) . .
C16 Si C17 106.7(3) . .
N1 Si C18 111.3(2) . .
C16 Si C18 108.5(3) . .
C17 Si C18 108.7(3) . .
C1 N1 Si 132.7(3) . .
C1 N1 K 92.4(3) . .
Si N1 K 118.7(2) . .
C3 N2 K 132.2(4) . 3
C3 N2 K 87.5(3) . .
K N2 K 101.07(13) 3 .
C19 N3 C22 108.6(8) . .
C19 N3 C21 109.9(9) . .
C22 N3 C21 108.7(8) . .
C19 N3 K 109.3(4) . .
C22 N3 K 106.2(4) . .
C21 N3 K 114.0(4) . .
C23 N4 C20 111.1(8) . .
C23 N4 C24 109.5(9) . .
C20 N4 C24 111.0(7) . .
C23 N4 K 110.9(5) . .
C20 N4 K 113.1(4) . .
C24 N4 K 100.8(5) . .
N1 C1 C2 124.0(4) . .
N1 C1 C4 120.2(4) . .
C2 C1 C4 115.8(4) . .
C1 C2 C3 125.8(4) . .
N2 C3 C2 127.2(5) . .
N2 C3 C10 116.3(4) . .
C2 C3 C10 116.5(4) . .
C9 C4 C5 117.5(5) . .
C9 C4 C1 122.2(5) . .
C5 C4 C1 120.3(5) . .
C6 C5 C4 121.6(5) . .
C5 C6 C7 119.6(6) . .
C8 C7 C6 119.7(5) . .
C7 C8 C9 120.0(5) . .
C4 C9 C8 121.5(5) . .
C15 C10 C11 118.1(5) . .
C15 C10 C3 122.1(4) . .
C11 C10 C3 119.8(4) . .
C12 C11 C10 119.8(5) . .
C13 C12 C11 121.1(5) . .
C12 C13 C14 119.7(5) . .
C13 C14 C15 119.8(5) . .
C10 C15 C14 121.5(5) . .
C20 C19 N3 130.2(8) . .
C19 C20 N4 122.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K N2 2.747(4) 3
K N4 2.775(5) .
K N3 2.831(5) .
K N1 2.889(4) .
K N2 2.993(5) .
Si N1 1.702(4) .
Si C16 1.869(5) .
Si C17 1.871(5) .
Si C18 1.871(5) .
N1 C1 1.326(6) .
N2 C3 1.303(6) .
N2 K 2.747(4) 3
N3 C19 1.391(9) .
N3 C22 1.401(9) .
N3 C21 1.403(9) .
N4 C23 1.416(10) .
N4 C20 1.436(8) .
N4 C24 1.444(10) .
C1 C2 1.381(6) .
C1 C4 1.512(6) .
C2 C3 1.436(6) .
C3 C10 1.489(7) .
C4 C9 1.375(7) .
C4 C5 1.385(7) .
C5 C6 1.378(7) .
C6 C7 1.381(8) .
C7 C8 1.366(8) .
C8 C9 1.384(7) .
C10 C15 1.378(6) .
C10 C11 1.397(6) .
C11 C12 1.381(7) .
C12 C13 1.367(7) .
C13 C14 1.370(8) .
C14 C15 1.379(7) .
C19 C20 1.320(10) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139184976
