#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:17:36 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223299 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/15/7701548.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_7701548
loop_
_publ_author_name
'Schüler, Philipp'
'Görls, Helmar'
'Westerhausen, Matthias'
'Krieck, Sven'
_publ_section_title
;
 Bis(trimethylsilyl)amide complexes of s-block metals with bidentate ether
 and amine ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8966
_journal_page_last               8975
_journal_paper_doi               10.1039/c9dt01426h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H56 K2 N2 O4 Si4'
_chemical_formula_sum            'C20 H56 K2 N2 O4 Si4'
_chemical_formula_weight         579.23
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-97
_audit_update_record
;
2019-04-01 deposited with the CCDC.	2019-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                106.864(2)
_cell_angle_beta                 102.532(1)
_cell_angle_gamma                109.884(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9461(3)
_cell_length_b                   10.7526(4)
_cell_length_c                   10.9069(4)
_cell_measurement_reflns_used    10528
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.29
_cell_volume                     884.21(6)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10528
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.427
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         4002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0262P)²+0.6666P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                3717
_reflns_number_total             4002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt01426h2.cif
_cod_data_source_block           FO6409
_cod_original_cell_volume        884.21(5)
_cod_database_code               7701548
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
K1 K 0.58965(4) 0.69628(3) 0.51605(3) 0.02177(9) Uani 1 1 d .
Si1 Si 0.64388(5) 0.41748(4) 0.27180(4) 0.01835(10) Uani 1 1 d .
Si2 Si 0.28065(5) 0.39898(5) 0.19583(4) 0.02056(10) Uani 1 1 d .
O1 O 0.7160(2) 0.92290(14) 0.44046(14) 0.0452(4) Uani 1 1 d .
O2 O 0.6990(2) 0.97625(13) 0.70229(13) 0.0467(4) Uani 1 1 d .
N1 N 0.47014(15) 0.42929(13) 0.29603(12) 0.0183(2) Uani 1 1 d .
C1 C 0.7252(2) 0.3240(2) 0.37406(18) 0.0297(4) Uani 1 1 d .
H1A H 0.6355 0.2280 0.3488 0.045 Uiso 1 1 calc R
H1B H 0.7587 0.3808 0.4719 0.045 Uiso 1 1 calc R
H1C H 0.8236 0.3147 0.3544 0.045 Uiso 1 1 calc R
C2 C 0.6249(2) 0.3197(2) 0.09075(17) 0.0327(4) Uani 1 1 d .
H2A H 0.5384 0.2201 0.0546 0.049 Uiso 1 1 calc R
H2B H 0.7344 0.3200 0.0900 0.049 Uiso 1 1 calc R
H2C H 0.5922 0.3683 0.0337 0.049 Uiso 1 1 calc R
C3 C 0.8308(2) 0.59830(18) 0.33307(18) 0.0296(3) Uani 1 1 d .
H3A H 0.8004 0.6545 0.2841 0.044 Uiso 1 1 calc R
H3B H 0.9277 0.5839 0.3154 0.044 Uiso 1 1 calc R
H3C H 0.8611 0.6503 0.4315 0.044 Uiso 1 1 calc R
C4 C 0.2500(2) 0.5687(2) 0.21603(18) 0.0340(4) Uani 1 1 d .
H4A H 0.3372 0.6336 0.1941 0.051 Uiso 1 1 calc R
H4B H 0.2596 0.6167 0.3106 0.051 Uiso 1 1 calc R
H4C H 0.1374 0.5436 0.1538 0.051 Uiso 1 1 calc R
C5 C 0.2230(2) 0.3048(2) 0.00580(17) 0.0355(4) Uani 1 1 d .
H5A H 0.3081 0.3609 -0.0242 0.053 Uiso 1 1 calc R
H5B H 0.1113 0.2959 -0.0421 0.053 Uiso 1 1 calc R
H5C H 0.2197 0.2087 -0.0151 0.053 Uiso 1 1 calc R
C6 C 0.1023(2) 0.2867(2) 0.23958(19) 0.0331(4) Uani 1 1 d .
H6A H 0.1057 0.1941 0.2285 0.050 Uiso 1 1 calc R
H6B H -0.0069 0.2701 0.1783 0.050 Uiso 1 1 calc R
H6C H 0.1157 0.3379 0.3345 0.050 Uiso 1 1 calc R
C7 C 0.7629(3) 1.06021(19) 0.5322(2) 0.0457(5) Uani 1 1 d .
H7A H 0.6676 1.0864 0.5097 0.055 Uiso 1 1 calc R
H7B H 0.8603 1.1277 0.5201 0.055 Uiso 1 1 calc R
C8 C 0.8094(3) 1.0803(2) 0.6750(2) 0.0469(5) Uani 1 1 d .
H8A H 0.9235 1.0829 0.7052 0.056 Uiso 1 1 calc R
H8B H 0.8175 1.1751 0.7299 0.056 Uiso 1 1 calc R
C9 C 0.7278(3) 1.0082(2) 0.84290(19) 0.0443(5) Uani 1 1 d .
H9A H 0.7182 1.0977 0.8847 0.066 Uiso 1 1 calc R
H9B H 0.8418 1.0196 0.8882 0.066 Uiso 1 1 calc R
H9C H 0.6433 0.9293 0.8533 0.066 Uiso 1 1 calc R
C10 C 0.6862(3) 0.9072(2) 0.3032(2) 0.0460(5) Uani 1 1 d .
H10A H 0.7860 0.9768 0.2972 0.069 Uiso 1 1 calc R
H10B H 0.5873 0.9248 0.2706 0.069 Uiso 1 1 calc R
H10C H 0.6645 0.8093 0.2466 0.069 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 0.0000 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'
O O 0.0106 0.0060 '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
O1 K1 O2 60.62(4) . .
O1 K1 N1 154.54(4) . 2_666
O2 K1 N1 94.56(4) . 2_666
O1 K1 N1 111.36(4) . .
O2 K1 N1 171.17(4) . .
N1 K1 N1 93.76(3) 2_666 .
O1 K1 Si1 142.23(3) . 2_666
O2 K1 Si1 86.31(3) . 2_666
N1 K1 Si1 26.29(2) 2_666 2_666
N1 K1 Si1 99.93(3) . 2_666
O1 K1 Si1 100.94(3) . .
O2 K1 Si1 153.03(4) . .
N1 K1 Si1 100.03(3) 2_666 .
N1 K1 Si1 26.30(2) . .
Si1 K1 Si1 116.123(10) 2_666 .
O1 K1 Si2 137.05(3) . 2_666
O2 K1 Si2 88.49(3) . 2_666
N1 K1 Si2 25.96(3) 2_666 2_666
N1 K1 Si2 100.31(3) . 2_666
Si1 K1 Si2 50.243(10) 2_666 2_666
Si1 K1 Si2 94.765(12) . 2_666
O1 K1 Si2 104.06(3) . .
O2 K1 Si2 148.09(4) . .
N1 K1 Si2 100.41(3) 2_666 .
N1 K1 Si2 25.98(3) . .
Si1 K1 Si2 94.772(12) 2_666 .
Si1 K1 Si2 50.208(10) . .
Si2 K1 Si2 116.514(11) 2_666 .
O1 K1 K1 157.87(3) . 2_666
O2 K1 K1 141.44(3) . 2_666
N1 K1 K1 46.97(2) 2_666 2_666
N1 K1 K1 46.79(3) . 2_666
Si1 K1 K1 58.095(10) 2_666 2_666
Si1 K1 K1 58.028(10) . 2_666
Si2 K1 K1 58.284(11) 2_666 2_666
Si2 K1 K1 58.230(10) . 2_666
N1 Si1 C2 117.22(7) . .
N1 Si1 C3 113.58(7) . .
C2 Si1 C3 104.25(8) . .
N1 Si1 C1 111.44(7) . .
C2 Si1 C1 105.42(8) . .
C3 Si1 C1 103.70(8) . .
N1 Si1 K1 48.14(4) . 2_666
C2 Si1 K1 131.56(6) . 2_666
C3 Si1 K1 124.10(5) . 2_666
C1 Si1 K1 63.31(5) . 2_666
N1 Si1 K1 48.34(4) . .
C2 Si1 K1 149.40(6) . .
C3 Si1 K1 69.27(5) . .
C1 Si1 K1 105.16(6) . .
K1 Si1 K1 63.877(10) 2_666 .
N1 Si2 C5 116.96(7) . .
N1 Si2 C6 111.59(7) . .
C5 Si2 C6 105.54(8) . .
N1 Si2 C4 113.61(7) . .
C5 Si2 C4 104.17(8) . .
C6 Si2 C4 103.76(8) . .
N1 Si2 K1 47.47(4) . 2_666
C5 Si2 K1 132.73(7) . 2_666
C6 Si2 K1 64.18(6) . 2_666
C4 Si2 K1 123.06(6) . 2_666
N1 Si2 K1 47.69(4) . .
C5 Si2 K1 147.39(6) . .
C6 Si2 K1 107.04(6) . .
C4 Si2 K1 69.29(6) . .
K1 Si2 K1 63.486(11) 2_666 .
C7 O1 C10 114.86(15) . .
C7 O1 K1 118.42(11) . .
C10 O1 K1 123.50(12) . .
C8 O2 C9 114.71(15) . .
C8 O2 K1 114.36(12) . .
C9 O2 K1 121.30(12) . .
Si2 N1 Si1 135.75(8) . .
Si2 N1 K1 106.57(5) . 2_666
Si1 N1 K1 105.56(6) . 2_666
Si2 N1 K1 106.33(5) . .
Si1 N1 K1 105.36(5) . .
K1 N1 K1 86.24(3) 2_666 .
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si2 C4 H4A 109.5 . .
Si2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si2 C5 H5A 109.5 . .
Si2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
Si2 C6 H6A 109.5 . .
Si2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
O1 C7 C8 115.20(16) . .
O1 C7 H7A 108.5 . .
C8 C7 H7A 108.5 . .
O1 C7 H7B 108.5 . .
C8 C7 H7B 108.5 . .
H7A C7 H7B 107.5 . .
O2 C8 C7 114.76(17) . .
O2 C8 H8A 108.6 . .
C7 C8 H8A 108.6 . .
O2 C8 H8B 108.6 . .
C7 C8 H8B 108.6 . .
H8A C8 H8B 107.6 . .
O2 C9 H9A 109.5 . .
O2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O1 C10 H10A 109.5 . .
O1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.7553(13) .
K1 O2 2.7807(13) .
K1 N1 2.8107(12) 2_666
K1 N1 2.8187(12) .
K1 Si1 3.6354(5) 2_666
K1 Si1 3.6381(5) .
K1 Si2 3.6557(5) 2_666
K1 Si2 3.6579(5) .
K1 K1 3.8478(6) 2_666
Si1 N1 1.6718(12) .
Si1 C2 1.8875(16) .
Si1 C3 1.8901(17) .
Si1 C1 1.8923(16) .
Si1 K1 3.6355(5) 2_666
Si2 N1 1.6697(12) .
Si2 C5 1.8842(17) .
Si2 C6 1.8934(17) .
Si2 C4 1.8938(18) .
Si2 K1 3.6557(5) 2_666
O1 C7 1.377(2) .
O1 C10 1.410(2) .
O2 C8 1.373(2) .
O2 C9 1.414(2) .
N1 K1 2.8107(12) 2_666
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.451(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
