#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:17:36 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223299 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/15/7701549.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_7701549
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 N2 O4 Rb2 Si4'
_chemical_formula_sum            'C20 H56 N2 O4 Rb2 Si4'
_chemical_formula_weight         671.97
_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                108.386(2)
_cell_angle_beta                 108.706(2)
_cell_angle_gamma                101.031(1)
_cell_formula_units_Z            1
_cell_length_a                   8.5102(3)
_cell_length_b                   11.0496(3)
_cell_length_c                   11.1416(3)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.64
_cell_volume                     890.44(5)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7116
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         4038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0263
_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)+(0.0106P)²+0.7064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                3763
_reflns_number_total             4038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt01426h2.cif
_cod_data_source_block           FO6535
_cod_database_code               7701549
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
Rb1 Rb 0.60763(3) 0.525383(17) 0.363227(19) 0.02456(6) Uani 1 1 d .
Si1 Si 0.27677(7) 0.19346(5) 0.29374(5) 0.02232(11) Uani 1 1 d .
Si2 Si 0.65134(7) 0.26285(5) 0.51065(5) 0.02034(11) Uani 1 1 d .
O1 O 0.6468(2) 0.36370(16) 0.11644(17) 0.0394(4) Uani 1 1 d .
O2 O 0.7691(2) 0.64212(16) 0.20831(16) 0.0387(4) Uani 1 1 d .
N1 N 0.4739(2) 0.29014(14) 0.42017(16) 0.0210(3) Uani 1 1 d .
C1 C 0.2001(3) 0.2771(2) 0.1715(2) 0.0357(5) Uani 1 1 d .
H1A H 0.2792 0.2854 0.1250 0.053 Uiso 1 1 calc R
H1B H 0.2005 0.3670 0.2242 0.053 Uiso 1 1 calc R
H1C H 0.0809 0.2223 0.1020 0.053 Uiso 1 1 calc R
C2 C 0.0970(3) 0.1617(2) 0.3560(3) 0.0399(5) Uani 1 1 d .
H2A H 0.1292 0.1201 0.4220 0.060 Uiso 1 1 calc R
H2B H -0.0129 0.1012 0.2767 0.060 Uiso 1 1 calc R
H2C H 0.0815 0.2475 0.4015 0.060 Uiso 1 1 calc R
C3 C 0.2574(3) 0.0194(2) 0.1789(3) 0.0424(6) Uani 1 1 d .
H3A H 0.2805 -0.0339 0.2342 0.064 Uiso 1 1 calc R
H3B H 0.3428 0.0264 0.1378 0.064 Uiso 1 1 calc R
H3C H 0.1386 -0.0247 0.1051 0.064 Uiso 1 1 calc R
C4 C 0.8594(3) 0.3857(2) 0.5354(2) 0.0282(4) Uani 1 1 d .
H4A H 0.8596 0.3748 0.4447 0.042 Uiso 1 1 calc R
H4B H 0.9614 0.3677 0.5893 0.042 Uiso 1 1 calc R
H4C H 0.8648 0.4781 0.5851 0.042 Uiso 1 1 calc R
C5 C 0.6741(3) 0.0915(2) 0.4364(2) 0.0320(4) Uani 1 1 d .
H5A H 0.6715 0.0735 0.3437 0.048 Uiso 1 1 calc R
H5B H 0.5769 0.0224 0.4301 0.048 Uiso 1 1 calc R
H5C H 0.7856 0.0897 0.4967 0.048 Uiso 1 1 calc R
C6 C 0.6802(3) 0.2931(2) 0.6951(2) 0.0298(4) Uani 1 1 d .
H6A H 0.5723 0.2409 0.6938 0.045 Uiso 1 1 calc R
H6B H 0.7054 0.3893 0.7482 0.045 Uiso 1 1 calc R
H6C H 0.7779 0.2647 0.7385 0.045 Uiso 1 1 calc R
C7 C 0.6502(4) 0.2338(3) 0.1119(3) 0.0562(7) Uani 1 1 d .
H7A H 0.6217 0.1728 0.0166 0.084 Uiso 1 1 calc R
H7B H 0.5639 0.1980 0.1433 0.084 Uiso 1 1 calc R
H7C H 0.7675 0.2414 0.1726 0.084 Uiso 1 1 calc R
C8 C 0.7813(3) 0.4267(3) 0.0865(2) 0.0400(5) Uani 1 1 d .
H8A H 0.7744 0.3664 -0.0036 0.048 Uiso 1 1 calc R
H8B H 0.8971 0.4439 0.1590 0.048 Uiso 1 1 calc R
C9 C 0.7632(3) 0.5565(3) 0.0808(2) 0.0404(5) Uani 1 1 d .
H9A H 0.8594 0.6011 0.0619 0.048 Uiso 1 1 calc R
H9B H 0.6504 0.5387 0.0046 0.048 Uiso 1 1 calc R
C10 C 0.7789(4) 0.7746(3) 0.2164(3) 0.0537(7) Uani 1 1 d .
H10A H 0.8835 0.8137 0.2046 0.080 Uiso 1 1 calc R
H10B H 0.7858 0.8307 0.3070 0.080 Uiso 1 1 calc R
H10C H 0.6740 0.7706 0.1430 0.080 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'
Rb Rb -0.9393 2.9676 '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 Rb1 O2 56.19(5) . .
O1 Rb1 N1 94.43(4) . .
O2 Rb1 N1 150.10(4) . .
O1 Rb1 N1 169.17(4) . 2_666
O2 Rb1 N1 118.05(4) . 2_666
N1 Rb1 N1 91.84(4) . 2_666
O1 Rb1 Si1 158.97(3) . 2_666
O2 Rb1 Si1 107.22(3) . 2_666
N1 Rb1 Si1 99.77(3) . 2_666
N1 Rb1 Si1 25.53(3) 2_666 2_666
O1 Rb1 Si2 144.23(3) . 2_666
O2 Rb1 Si2 109.05(3) . 2_666
N1 Rb1 Si2 98.34(3) . 2_666
N1 Rb1 Si2 25.40(3) 2_666 2_666
Si1 Rb1 Si2 48.447(11) 2_666 2_666
O1 Rb1 Si2 91.74(3) . .
O2 Rb1 Si2 136.80(3) . .
N1 Rb1 Si2 25.13(3) . .
N1 Rb1 Si2 97.66(3) 2_666 .
Si1 Rb1 Si2 94.561(12) 2_666 .
Si2 Rb1 Si2 113.265(10) 2_666 .
O1 Rb1 Si1 84.93(3) . .
O2 Rb1 Si1 138.17(3) . .
N1 Rb1 Si1 24.20(3) . .
N1 Rb1 Si1 97.39(3) 2_666 .
Si1 Rb1 Si1 113.952(9) 2_666 .
Si2 Rb1 Si1 93.285(12) 2_666 .
Si2 Rb1 Si1 47.753(11) . .
O1 Rb1 Rb1 139.82(3) . 2_666
O2 Rb1 Rb1 163.72(3) . 2_666
N1 Rb1 Rb1 46.16(3) . 2_666
N1 Rb1 Rb1 45.68(3) 2_666 2_666
Si1 Rb1 Rb1 58.014(9) 2_666 2_666
Si2 Rb1 Rb1 56.763(9) 2_666 2_666
Si2 Rb1 Rb1 56.502(9) . 2_666
Si1 Rb1 Rb1 55.938(9) . 2_666
N1 Si1 C3 117.11(9) . .
N1 Si1 C2 114.29(9) . .
C3 Si1 C2 103.73(11) . .
N1 Si1 C1 110.60(9) . .
C3 Si1 C1 105.10(11) . .
C2 Si1 C1 104.88(11) . .
N1 Si1 Rb1 50.62(5) . 2_666
C3 Si1 Rb1 154.27(9) . 2_666
C2 Si1 Rb1 70.01(8) . 2_666
C1 Si1 Rb1 100.61(7) . 2_666
N1 Si1 Rb1 46.84(5) . .
C3 Si1 Rb1 125.45(8) . .
C2 Si1 Rb1 130.80(8) . .
C1 Si1 Rb1 63.99(7) . .
Rb1 Si1 Rb1 66.049(9) 2_666 .
N1 Si2 C5 117.43(9) . .
N1 Si2 C4 111.22(9) . .
C5 Si2 C4 104.46(9) . .
N1 Si2 C6 113.74(9) . .
C5 Si2 C6 105.49(10) . .
C4 Si2 C6 103.16(9) . .
N1 Si2 Rb1 50.43(5) . 2_666
C5 Si2 Rb1 149.52(7) . 2_666
C4 Si2 Rb1 106.01(7) . 2_666
C6 Si2 Rb1 66.65(7) . 2_666
N1 Si2 Rb1 49.20(5) . .
C5 Si2 Rb1 130.88(7) . .
C4 Si2 Rb1 62.03(6) . .
C6 Si2 Rb1 123.33(6) . .
Rb1 Si2 Rb1 66.735(10) 2_666 .
C8 O1 C7 112.04(19) . .
C8 O1 Rb1 116.78(13) . .
C7 O1 Rb1 112.13(14) . .
C9 O2 C10 112.36(19) . .
C9 O2 Rb1 119.79(13) . .
C10 O2 Rb1 121.62(15) . .
Si2 N1 Si1 135.62(9) . .
Si2 N1 Rb1 105.67(7) . .
Si1 N1 Rb1 108.95(7) . .
Si2 N1 Rb1 104.17(7) . 2_666
Si1 N1 Rb1 103.85(7) . 2_666
Rb1 N1 Rb1 88.16(4) . 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 H7A 109.5 . .
O1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O1 C8 C9 110.03(18) . .
O1 C8 H8A 109.7 . .
C9 C8 H8A 109.7 . .
O1 C8 H8B 109.7 . .
C9 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
O2 C9 C8 110.00(18) . .
O2 C9 H9A 109.7 . .
C8 C9 H9A 109.7 . .
O2 C9 H9B 109.7 . .
C8 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
O2 C10 H10A 109.5 . .
O2 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O2 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
Rb1 O1 2.9291(15) .
Rb1 O2 2.9627(15) .
Rb1 N1 2.9709(15) .
Rb1 N1 2.9952(15) 2_666
Rb1 Si1 3.7622(5) 2_666
Rb1 Si2 3.7674(5) 2_666
Rb1 Si2 3.7787(5) .
Rb1 Si1 3.8519(5) .
Rb1 Rb1 4.1504(4) 2_666
Si1 N1 1.6698(16) .
Si1 C3 1.885(2) .
Si1 C2 1.890(2) .
Si1 C1 1.895(2) .
Si1 Rb1 3.7623(5) 2_666
Si2 N1 1.6667(16) .
Si2 C5 1.887(2) .
Si2 C4 1.893(2) .
Si2 C6 1.899(2) .
Si2 Rb1 3.7674(5) 2_666
O1 C8 1.412(3) .
O1 C7 1.426(3) .
O2 C9 1.416(3) .
O2 C10 1.422(3) .
N1 Rb1 2.9952(15) 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 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.490(3) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
