#------------------------------------------------------------------------------
#$Date: 2025-08-21 16:09:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301850 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/64/7046402.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_7046402
loop_
_publ_author_name
'Krieck, Sven'
'Schüler, Philipp'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Straightforward synthesis of rubidium bis(trimethylsilyl)amide and
 complexes of the alkali metal bis(trimethylsilyl)amides with weakly
 coordinating 2,2,5,5-tetramethyltetrahydrofuran.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12562
_journal_page_last               12569
_journal_paper_doi               10.1039/c8dt01539b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H52 N2 O2 Rb2 Si4'
_chemical_formula_sum            'C20 H52 N2 O2 Rb2 Si4'
_chemical_formula_weight         635.94
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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-97
_audit_update_record
;
2018-04-18 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.229(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1879(2)
_cell_length_b                   12.3031(2)
_cell_length_c                   12.5560(2)
_cell_measurement_reflns_used    12950
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.73
_cell_volume                     1667.59(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12950
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0258
_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)+(0.0129P)²+1.5434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                3386
_reflns_number_total             3761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01539b2.cif
_cod_data_source_block           FO6563
_cod_depositor_comments
'Adding full bibliography for 7046399--7046403.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7046402
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
Rb1 Rb 0.483816(16) 0.558099(15) 0.349951(14) 0.02193(6) Uani 1 1 d .
Si1 Si 0.38949(5) 0.26891(4) 0.39089(4) 0.02167(11) Uani 1 1 d .
Si2 Si 0.21300(5) 0.43085(4) 0.44815(4) 0.02086(11) Uani 1 1 d .
O1 O 0.59873(15) 0.55192(13) 0.17369(13) 0.0373(4) Uani 1 1 d .
N1 N 0.34856(14) 0.39097(13) 0.42817(13) 0.0221(3) Uani 1 1 d .
C1 C 0.4810(2) 0.27751(18) 0.28458(17) 0.0321(5) Uani 1 1 d .
H1A H 0.5608 0.3127 0.3172 0.048 Uiso 1 1 calc R
H1B H 0.4345 0.3201 0.2213 0.048 Uiso 1 1 calc R
H1C H 0.4951 0.2041 0.2601 0.048 Uiso 1 1 calc R
C2 C 0.4914(2) 0.19042(17) 0.51001(17) 0.0305(4) Uani 1 1 d .
H2A H 0.5710 0.2279 0.5365 0.046 Uiso 1 1 calc R
H2B H 0.5055 0.1171 0.4853 0.046 Uiso 1 1 calc R
H2C H 0.4506 0.1856 0.5700 0.046 Uiso 1 1 calc R
C3 C 0.25547(19) 0.17597(18) 0.32465(18) 0.0322(5) Uani 1 1 d .
H3A H 0.2072 0.2082 0.2553 0.048 Uiso 1 1 calc R
H3B H 0.2023 0.1665 0.3748 0.048 Uiso 1 1 calc R
H3C H 0.2876 0.1051 0.3096 0.048 Uiso 1 1 calc R
C4 C 0.1716(2) 0.35703(19) 0.56557(17) 0.0323(5) Uani 1 1 d .
H4A H 0.1678 0.2787 0.5509 0.048 Uiso 1 1 calc R
H4B H 0.0907 0.3823 0.5721 0.048 Uiso 1 1 calc R
H4C H 0.2346 0.3718 0.6346 0.048 Uiso 1 1 calc R
C5 C 0.07269(19) 0.41677(19) 0.32662(17) 0.0318(5) Uani 1 1 d .
H5A H 0.0546 0.3396 0.3112 0.048 Uiso 1 1 calc R
H5B H 0.0892 0.4515 0.2617 0.048 Uiso 1 1 calc R
H5C H 0.0014 0.4519 0.3438 0.048 Uiso 1 1 calc R
C6 C 0.21840(19) 0.58027(17) 0.48436(18) 0.0303(4) Uani 1 1 d .
H6A H 0.2235 0.6234 0.4201 0.045 Uiso 1 1 calc R
H6B H 0.2913 0.5948 0.5457 0.045 Uiso 1 1 calc R
H6C H 0.1433 0.6001 0.5060 0.045 Uiso 1 1 calc R
C7 C 0.6866(2) 0.46999(19) 0.1640(2) 0.0412(6) Uani 1 1 d .
H7A H 0.6432 0.4037 0.1291 0.049 Uiso 1 1 calc R
H7B H 0.7400 0.4505 0.2377 0.049 Uiso 1 1 calc R
C8 C 0.7627(3) 0.5174(2) 0.0937(3) 0.0552(7) Uani 1 1 d .
H8A H 0.8389 0.5517 0.1397 0.066 Uiso 1 1 calc R
H8B H 0.7859 0.4610 0.0465 0.066 Uiso 1 1 calc R
C9 C 0.6790(3) 0.5997(3) 0.0260(2) 0.0555(8) Uani 1 1 d .
H9A H 0.6226 0.5661 -0.0399 0.067 Uiso 1 1 calc R
H9B H 0.7267 0.6584 0.0021 0.067 Uiso 1 1 calc R
C10 C 0.6086(3) 0.6419(2) 0.1042(2) 0.0489(6) Uani 1 1 d .
H10A H 0.6538 0.7029 0.1487 0.059 Uiso 1 1 calc R
H10B H 0.5255 0.6677 0.0632 0.059 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 N1 129.37(5) . .
O1 Rb1 N1 115.52(5) . 3_666
N1 Rb1 N1 95.12(4) . 3_666
O1 Rb1 Si2 90.79(4) . 3_666
N1 Rb1 Si2 105.36(3) . 3_666
N1 Rb1 Si2 26.75(3) 3_666 3_666
O1 Rb1 Si1 106.28(3) . .
N1 Rb1 Si1 24.56(3) . .
N1 Rb1 Si1 101.52(3) 3_666 .
Si2 Rb1 Si1 100.450(12) 3_666 .
O1 Rb1 Si1 122.31(4) . 3_666
N1 Rb1 Si1 102.56(3) . 3_666
N1 Rb1 Si1 24.60(3) 3_666 3_666
Si2 Rb1 Si1 47.454(12) 3_666 3_666
Si1 Rb1 Si1 117.430(9) . 3_666
O1 Rb1 Si2 141.92(4) . .
N1 Rb1 Si2 23.00(3) . .
N1 Rb1 Si2 98.01(3) 3_666 .
Si2 Rb1 Si2 116.895(9) 3_666 .
Si1 Rb1 Si2 46.365(11) . .
Si1 Rb1 Si2 95.713(11) 3_666 .
O1 Rb1 Rb1 141.83(3) . 3_666
N1 Rb1 Rb1 48.77(3) . 3_666
N1 Rb1 Rb1 46.35(3) 3_666 3_666
Si2 Rb1 Rb1 61.195(9) 3_666 3_666
Si1 Rb1 Rb1 59.336(9) . 3_666
Si1 Rb1 Rb1 58.094(9) 3_666 3_666
Si2 Rb1 Rb1 55.700(9) . 3_666
N1 Si1 C1 112.77(9) . .
N1 Si1 C2 112.95(9) . .
C1 Si1 C2 105.18(10) . .
N1 Si1 C3 114.92(9) . .
C1 Si1 C3 103.71(10) . .
C2 Si1 C3 106.39(10) . .
N1 Si1 Rb1 45.60(5) . .
C1 Si1 Rb1 68.20(7) . .
C2 Si1 Rb1 117.13(7) . .
C3 Si1 Rb1 136.41(7) . .
N1 Si1 Rb1 48.04(6) . 3_666
C1 Si1 Rb1 114.90(7) . 3_666
C2 Si1 Rb1 66.45(7) . 3_666
C3 Si1 Rb1 141.33(7) . 3_666
Rb1 Si1 Rb1 62.570(9) . 3_666
N1 Si2 C5 116.46(9) . .
N1 Si2 C4 113.17(9) . .
C5 Si2 C4 105.32(10) . .
N1 Si2 C6 110.36(9) . .
C5 Si2 C6 104.52(10) . .
C4 Si2 C6 106.17(10) . .
N1 Si2 Rb1 53.44(6) . 3_666
C5 Si2 Rb1 169.87(7) . 3_666
C4 Si2 Rb1 81.40(7) . 3_666
C6 Si2 Rb1 80.35(7) . 3_666
N1 Si2 Rb1 42.14(6) . .
C5 Si2 Rb1 109.41(7) . .
C4 Si2 Rb1 144.31(7) . .
C6 Si2 Rb1 72.92(7) . .
Rb1 Si2 Rb1 63.105(9) 3_666 .
C10 O1 C7 109.11(17) . .
C10 O1 Rb1 125.29(14) . .
C7 O1 Rb1 123.07(13) . .
Si1 N1 Si2 129.08(10) . .
Si1 N1 Rb1 109.83(7) . .
Si2 N1 Rb1 114.86(8) . .
Si1 N1 Rb1 107.36(7) . 3_666
Si2 N1 Rb1 99.80(7) . 3_666
Rb1 N1 Rb1 84.88(4) . 3_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 106.54(19) . .
O1 C7 H7A 110.4 . .
C8 C7 H7A 110.4 . .
O1 C7 H7B 110.4 . .
C8 C7 H7B 110.4 . .
H7A C7 H7B 108.6 . .
C9 C8 C7 103.5(2) . .
C9 C8 H8A 111.1 . .
C7 C8 H8A 111.1 . .
C9 C8 H8B 111.1 . .
C7 C8 H8B 111.1 . .
H8A C8 H8B 109.0 . .
C8 C9 C10 102.7(2) . .
C8 C9 H9A 111.2 . .
C10 C9 H9A 111.2 . .
C8 C9 H9B 111.2 . .
C10 C9 H9B 111.2 . .
H9A C9 H9B 109.1 . .
O1 C10 C9 105.6(2) . .
O1 C10 H10A 110.6 . .
C9 C10 H10A 110.6 . .
O1 C10 H10B 110.6 . .
C9 C10 H10B 110.6 . .
H10A C10 H10B 108.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 O1 2.8375(15) .
Rb1 N1 2.8746(16) .
Rb1 N1 2.9876(16) 3_666
Rb1 Si2 3.6651(5) 3_666
Rb1 Si1 3.7845(6) .
Rb1 Si1 3.8346(5) 3_666
Rb1 Si2 3.8877(5) .
Rb1 Rb1 3.9568(3) 3_666
Si1 N1 1.6723(17) .
Si1 C1 1.886(2) .
Si1 C2 1.890(2) .
Si1 C3 1.895(2) .
Si1 Rb1 3.8346(5) 3_666
Si2 N1 1.6744(16) .
Si2 C5 1.888(2) .
Si2 C4 1.890(2) .
Si2 C6 1.891(2) .
Si2 Rb1 3.6651(5) 3_666
O1 C10 1.432(3) .
O1 C7 1.435(3) .
N1 Rb1 2.9877(16) 3_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 1.496(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.485(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.504(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139172768
