#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/04/7010424.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_7010424
loop_
_publ_author_name
'Liddle, Stephen T.'
'Clegg, William'
_publ_section_title
;
 Cation-induced structural variations in the alkali metal derivatives
 of 2-trimethylsilylaminopyridine: synthesis and X-ray structures of
 complexes for all five metals Li--Cs with 12-crown-4 †
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              402
_journal_paper_doi               10.1039/b008852h
_journal_year                    2001
_chemical_formula_sum            'C32 H58 N4 O8 Rb2 Si2'
_chemical_formula_weight         853.94
_space_group_IT_number           2
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.949(2)
_cell_angle_beta                 108.155(2)
_cell_angle_gamma                91.402(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8861(15)
_cell_length_b                   10.0654(15)
_cell_length_c                   11.9755(17)
_cell_measurement_reflns_used    6778
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.36
_cell_volume                     1074.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7660
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.379
_exptl_absorpt_correction_T_max  0.449
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0534
_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)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                2783
_reflns_number_total             3719
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b008852h.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010424
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.58266(5) 0.67880(4) 0.58879(4) 0.0433(2) Uani 1 1 d . . .
N1 N 0.6937(4) 0.4191(4) 0.6491(3) 0.0371(9) Uani 1 1 d . . .
N2 N 0.4750(4) 0.4604(4) 0.6752(3) 0.0393(9) Uani 1 1 d . . .
C1 C 0.8302(5) 0.3966(5) 0.6945(5) 0.0449(12) Uani 1 1 d U . .
H1 H 0.8863 0.3838 0.6414 0.054 Uiso 1 1 calc R . .
C2 C 0.8957(5) 0.3906(5) 0.8138(5) 0.0527(13) Uani 1 1 d U . .
H2 H 0.9925 0.3730 0.8411 0.063 Uiso 1 1 calc R . .
C3 C 0.8139(5) 0.4115(5) 0.8909(5) 0.0508(12) Uani 1 1 d U . .
H3 H 0.8545 0.4091 0.9733 0.061 Uiso 1 1 calc R . .
C4 C 0.6757(5) 0.4354(5) 0.8489(4) 0.0424(11) Uani 1 1 d U . .
H4 H 0.6207 0.4499 0.9028 0.051 Uiso 1 1 calc R . .
C5 C 0.6106(5) 0.4393(4) 0.7251(4) 0.0338(10) Uani 1 1 d U . .
Si1 Si 0.34164(15) 0.48364(16) 0.73600(12) 0.0465(4) Uani 1 1 d . . .
C6 C 0.1817(6) 0.5008(8) 0.6114(5) 0.0728(18) Uani 1 1 d . . .
H6A H 0.2036 0.5793 0.5844 0.109 Uiso 1 1 calc R . .
H6B H 0.1013 0.5180 0.6430 0.109 Uiso 1 1 calc R . .
H6C H 0.1557 0.4142 0.5412 0.109 Uiso 1 1 calc R . .
C7 C 0.2924(6) 0.3323(7) 0.7838(6) 0.0688(17) Uani 1 1 d . . .
H7A H 0.2669 0.2465 0.7127 0.103 Uiso 1 1 calc R . .
H7B H 0.2103 0.3503 0.8129 0.103 Uiso 1 1 calc R . .
H7C H 0.3742 0.3212 0.8505 0.103 Uiso 1 1 calc R . .
C8 C 0.3764(7) 0.6470(6) 0.8717(5) 0.0670(17) Uani 1 1 d . . .
H8A H 0.4664 0.6465 0.9360 0.100 Uiso 1 1 calc R . .
H8B H 0.2973 0.6505 0.9050 0.100 Uiso 1 1 calc R . .
H8C H 0.3838 0.7292 0.8449 0.100 Uiso 1 1 calc R . .
O1 O 0.8338(11) 0.8685(8) 0.5905(8) 0.167(3) Uani 1 1 d . . .
O2 O 0.9281(11) 0.8768(8) 0.8334(8) 0.181(4) Uani 1 1 d . . .
O3 O 0.6402(15) 0.8755(8) 0.8525(9) 0.238(6) Uani 1 1 d . . .
O4 O 0.5903(8) 0.9733(5) 0.6498(7) 0.153(3) Uani 1 1 d . . .
C9 C 0.931(2) 0.948(3) 0.6591(17) 0.319(12) Uani 1 1 d U . .
H9A H 0.9056 1.0340 0.7092 0.383 Uiso 1 1 calc R . .
H9B H 1.0011 0.9699 0.6213 0.383 Uiso 1 1 calc R . .
C10 C 0.9816(14) 0.8176(15) 0.7394(15) 0.250(10) Uani 1 1 d U . .
H10A H 0.9327 0.7222 0.6881 0.300 Uiso 1 1 calc R . .
H10B H 1.0867 0.8163 0.7700 0.300 Uiso 1 1 calc R . .
C11 C 0.871(2) 0.7941(10) 0.8973(14) 0.265(12) Uani 1 1 d U . .
H11A H 0.8177 0.7030 0.8390 0.319 Uiso 1 1 calc R . .
H11B H 0.9485 0.7781 0.9660 0.319 Uiso 1 1 calc R . .
C12 C 0.781(3) 0.8819(17) 0.9401(17) 0.300(12) Uani 1 1 d U . .
H12A H 0.8294 0.9793 0.9698 0.360 Uiso 1 1 calc R . .
H12B H 0.7695 0.8606 1.0124 0.360 Uiso 1 1 calc R . .
C13 C 0.6497(19) 1.0045(15) 0.8827(13) 0.223(6) Uani 1 1 d U . .
H13A H 0.7487 1.0464 0.9002 0.267 Uiso 1 1 calc R . .
H13B H 0.6205 1.0436 0.9564 0.267 Uiso 1 1 calc R . .
C14 C 0.5497(16) 1.0286(13) 0.7732(13) 0.195(6) Uani 1 1 d U . .
H14A H 0.5443 1.1305 0.7915 0.234 Uiso 1 1 calc R . .
H14B H 0.4530 0.9825 0.7574 0.234 Uiso 1 1 calc R . .
C15 C 0.6672(16) 1.0635(12) 0.6507(15) 0.196(7) Uani 1 1 d U . .
H15A H 0.7391 1.1075 0.7339 0.235 Uiso 1 1 calc R . .
H15B H 0.6137 1.1361 0.6225 0.235 Uiso 1 1 calc R . .
C16 C 0.7337(18) 0.9868(12) 0.5624(15) 0.193(6) Uani 1 1 d U . .
H16A H 0.7921 1.0570 0.5477 0.232 Uiso 1 1 calc R . .
H16B H 0.6553 0.9416 0.4832 0.232 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
_geom_angle_publ_flag
O4 Rb1 N2 112.96(18) . 2_666 ?
O4 Rb1 N2 134.8(2) . . ?
N2 Rb1 N2 104.06(9) 2_666 . ?
O4 Rb1 N1 150.88(14) . . ?
N2 Rb1 N1 90.98(10) 2_666 . ?
N2 Rb1 N1 44.94(10) . . ?
O4 Rb1 O3 56.3(3) . . ?
N2 Rb1 O3 169.2(2) 2_666 . ?
N2 Rb1 O3 85.72(15) . . ?
N1 Rb1 O3 99.3(3) . . ?
O4 Rb1 O1 57.6(3) . . ?
N2 Rb1 O1 88.89(16) 2_666 . ?
N2 Rb1 O1 150.0(2) . . ?
N1 Rb1 O1 109.2(2) . . ?
O3 Rb1 O1 84.57(19) . . ?
O4 Rb1 N1 100.64(13) . 2_666 ?
N2 Rb1 N1 44.50(10) 2_666 2_666 ?
N2 Rb1 N1 87.82(9) . 2_666 ?
N1 Rb1 N1 108.21(8) . 2_666 ?
O3 Rb1 N1 133.2(3) . 2_666 ?
O1 Rb1 N1 119.04(19) . 2_666 ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Rb1 128.2(3) . . ?
C5 N1 Rb1 85.7(2) . . ?
C1 N1 Rb1 142.8(3) . 2_666 ?
C5 N1 Rb1 91.0(2) . 2_666 ?
Rb1 N1 Rb1 71.79(8) . 2_666 ?
C5 N2 Si1 130.2(3) . . ?
C5 N2 Rb1 102.4(3) . 2_666 ?
Si1 N2 Rb1 121.54(17) . 2_666 ?
C5 N2 Rb1 89.1(3) . . ?
Si1 N2 Rb1 121.60(19) . . ?
Rb1 N2 Rb1 75.94(9) 2_666 . ?
N1 C1 C2 124.6(5) . . ?
C3 C2 C1 117.3(5) . . ?
C4 C3 C2 119.9(5) . . ?
C3 C4 C5 121.7(5) . . ?
N2 C5 N1 116.3(4) . . ?
N2 C5 C4 125.8(4) . . ?
N1 C5 C4 117.9(4) . . ?
N2 Si1 C6 106.1(2) . . ?
N2 Si1 C8 114.2(2) . . ?
C6 Si1 C8 107.1(3) . . ?
N2 Si1 C7 114.0(2) . . ?
C6 Si1 C7 107.3(3) . . ?
C8 Si1 C7 107.8(3) . . ?
C9 O1 C16 94.4(16) . . ?
C9 O1 Rb1 140.3(10) . . ?
C16 O1 Rb1 92.7(7) . . ?
C10 O2 C11 123.3(13) . . ?
C13 O3 C12 91.4(10) . . ?
C13 O3 Rb1 125.2(10) . . ?
C12 O3 Rb1 115.9(12) . . ?
C15 O4 C14 106.4(11) . . ?
C15 O4 Rb1 134.7(10) . . ?
C14 O4 Rb1 107.9(6) . . ?
O1 C9 C10 87.9(15) . . ?
O2 C10 C9 95.9(10) . . ?
C12 C11 O2 100.7(11) . . ?
C11 C12 O3 116.4(14) . . ?
O3 C13 C14 102.8(13) . . ?
C13 C14 O4 115.0(10) . . ?
O4 C15 C16 100.8(11) . . ?
C15 C16 O1 121.2(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O4 2.832(5) . ?
Rb1 N2 2.922(4) 2_666 ?
Rb1 N2 2.990(4) . ?
Rb1 N1 3.051(4) . ?
Rb1 O3 3.065(8) . ?
Rb1 O1 3.086(8) . ?
Rb1 N1 3.152(4) 2_666 ?
N1 C1 1.341(6) . ?
N1 C5 1.382(6) . ?
N1 Rb1 3.152(4) 2_666 ?
N2 C5 1.336(5) . ?
N2 Si1 1.684(4) . ?
N2 Rb1 2.922(4) 2_666 ?
C1 C2 1.393(7) . ?
C2 C3 1.382(7) . ?
C3 C4 1.354(7) . ?
C4 C5 1.434(6) . ?
Si1 C6 1.857(5) . ?
Si1 C8 1.878(6) . ?
Si1 C7 1.879(6) . ?
O1 C9 1.151(14) . ?
O1 C16 1.610(15) . ?
O2 C10 1.378(16) . ?
O2 C11 1.49(2) . ?
O3 C13 1.235(15) . ?
O3 C12 1.45(2) . ?
O4 C15 1.166(15) . ?
O4 C14 1.598(15) . ?
C9 C10 1.83(2) . ?
C11 C12 1.37(3) . ?
C13 C14 1.465(17) . ?
C15 C16 1.46(2) . ?
