#------------------------------------------------------------------------------
#$Date: 2023-04-20 09:45:28 +0300 (Thu, 20 Apr 2023) $
#$Revision: 282761 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556518.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_1556518
loop_
_publ_author_name
'Von Pilgrim, M.'
'Mondeshki, M.'
'Klett, J.'
_publ_section_title
;
 [Bis(Trimethylsilyl)Methyl]Lithium and -Sodium: Solubility in Alkanes and
 Complexes with O- and N- Donor Ligands
;
_journal_name_full               Inorganics
_journal_page_first              39
_journal_paper_doi               10.3390/inorganics5020039
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C32 H86 N6 Na2 Si4'
_chemical_formula_weight         713.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 100.824(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.450(4)
_cell_length_b                   17.414(6)
_cell_length_c                   14.258(5)
_cell_measurement_reflns_used    5619
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.8036
_cell_measurement_theta_min      2.2289
_cell_volume                     2548.5(16)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.929
_diffrn_reflns_theta_min         2.303
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.930
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6055
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0570P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3494
_reflns_number_total             6055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            2b.cif
_cod_data_source_block           jkm18
_cod_depositor_comments
;

2023-04-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C10.67 H28.67 N2 Na0.67 Si1.33'
_cod_original_formula_weight         237.80
_cod_original_formula_units_Z            6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1556518
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.47721(6) 0.37102(4) 0.78551(5) 0.03882(19) Uani 1 1 d . . . . .
C1 C 0.63644(18) 0.26734(10) 0.76199(14) 0.0371(4) Uani 1 1 d . . . . .
H1 H 0.7010(18) 0.2890(10) 0.8079(14) 0.042(5) Uiso 1 1 d . . . . .
Si11 Si 0.59886(5) 0.17345(3) 0.80373(4) 0.04154(15) Uani 1 1 d . . . . .
C111 C 0.7475(2) 0.11299(13) 0.85399(19) 0.0697(7) Uani 1 1 d . . . . .
H11G H 0.8021 0.1084 0.8071 0.104 Uiso 1 1 calc R U . . .
H11H H 0.7201 0.0628 0.8700 0.104 Uiso 1 1 calc R U . . .
H11I H 0.7955 0.1372 0.9103 0.104 Uiso 1 1 calc R U . . .
C112 C 0.4993(2) 0.11279(13) 0.70657(17) 0.0651(6) Uani 1 1 d . . . . .
H11D H 0.4222 0.1403 0.6781 0.098 Uiso 1 1 calc R U . . .
H11E H 0.4751 0.0657 0.7336 0.098 Uiso 1 1 calc R U . . .
H11F H 0.5500 0.1016 0.6587 0.098 Uiso 1 1 calc R U . . .
C113 C 0.5033(2) 0.17589(14) 0.90457(17) 0.0692(7) Uani 1 1 d . . . . .
H11A H 0.4255 0.2056 0.8853 0.104 Uiso 1 1 calc R U . . .
H11B H 0.5557 0.1988 0.9600 0.104 Uiso 1 1 calc R U . . .
H11C H 0.4804 0.1245 0.9193 0.104 Uiso 1 1 calc R U . . .
Si12 Si 0.68664(5) 0.27890(3) 0.64817(4) 0.04175(16) Uani 1 1 d . . . . .
C121 C 0.8118(2) 0.20691(13) 0.61925(18) 0.0630(6) Uani 1 1 d . . . . .
H12G H 0.8868 0.2070 0.6697 0.094 Uiso 1 1 calc R U . . .
H12H H 0.8373 0.2211 0.5604 0.094 Uiso 1 1 calc R U . . .
H12I H 0.7740 0.1565 0.6131 0.094 Uiso 1 1 calc R U . . .
C122 C 0.7667(2) 0.37537(12) 0.64004(19) 0.0642(6) Uani 1 1 d . . . . .
H12D H 0.7093 0.4154 0.6533 0.096 Uiso 1 1 calc R U . . .
H12E H 0.7846 0.3822 0.5770 0.096 Uiso 1 1 calc R U . . .
H12F H 0.8467 0.3776 0.6858 0.096 Uiso 1 1 calc R U . . .
C123 C 0.5454(2) 0.27200(14) 0.54310(16) 0.0649(6) Uani 1 1 d . . . . .
H12A H 0.4776 0.3067 0.5526 0.097 Uiso 1 1 calc R U . . .
H12B H 0.5122 0.2205 0.5382 0.097 Uiso 1 1 calc R U . . .
H12C H 0.5749 0.2853 0.4854 0.097 Uiso 1 1 calc R U . . .
N21 N 0.2316(7) 0.3459(3) 0.7592(5) 0.049(2) Uani 0.78 1 d D . P A 1
C21 C 0.1742(4) 0.3225(3) 0.8404(3) 0.0695(11) Uani 0.78 1 d D . P A 1
H21A H 0.0825 0.3139 0.8196 0.104 Uiso 0.78 1 calc R U P A 1
H21B H 0.1874 0.3623 0.8879 0.104 Uiso 0.78 1 calc R U P A 1
H21C H 0.2149 0.2761 0.8672 0.104 Uiso 0.78 1 calc R U P A 1
C22 C 0.2148(6) 0.2830(3) 0.6884(4) 0.0684(13) Uani 0.78 1 d D . P A 1
H22A H 0.1245 0.2689 0.6729 0.103 Uiso 0.78 1 calc R U P A 1
H22B H 0.2654 0.2394 0.7147 0.103 Uiso 0.78 1 calc R U P A 1
H22C H 0.2436 0.2999 0.6317 0.103 Uiso 0.78 1 calc R U P A 1
C23 C 0.1668(3) 0.41606(18) 0.7160(3) 0.0551(8) Uani 0.78 1 d D . P A 1
H23C H 0.1672 0.4543 0.7656 0.066 Uiso 0.78 1 calc R U P A 1
H23D H 0.0767 0.4043 0.6889 0.066 Uiso 0.78 1 calc R U P A 1
C24 C 0.2329(2) 0.4496(2) 0.6378(2) 0.0490(7) Uani 0.78 1 d D . P A 1
H24C H 0.2365 0.4104 0.5900 0.059 Uiso 0.78 1 calc R U P A 1
H24D H 0.1807 0.4918 0.6069 0.059 Uiso 0.78 1 calc R U P A 1
N22 N 0.3653(4) 0.4774(2) 0.6747(3) 0.0410(10) Uani 0.78 1 d D . P A 1
C25 C 0.3599(4) 0.5486(2) 0.7315(3) 0.0628(10) Uani 0.78 1 d D . P A 1
H25A H 0.3184 0.5886 0.6905 0.094 Uiso 0.78 1 calc R U P A 1
H25B H 0.4468 0.5641 0.7597 0.094 Uiso 0.78 1 calc R U P A 1
H25C H 0.3111 0.5389 0.7810 0.094 Uiso 0.78 1 calc R U P A 1
C26 C 0.4309(10) 0.4968(7) 0.5955(6) 0.058(2) Uani 0.78 1 d D . P A 1
H26A H 0.3834 0.5368 0.5577 0.087 Uiso 0.78 1 calc R U P A 1
H26B H 0.4343 0.4522 0.5565 0.087 Uiso 0.78 1 calc R U P A 1
H26C H 0.5178 0.5142 0.6205 0.087 Uiso 0.78 1 calc R U P A 1
N21A N 0.236(3) 0.3454(10) 0.7493(16) 0.051(8) Uiso 0.22 1 d D . P A 3
C21A C 0.163(3) 0.3519(11) 0.8276(15) 0.108(9) Uiso 0.22 1 d D . P A 3
H21D H 0.0716 0.3437 0.8031 0.162 Uiso 0.22 1 calc R U P A 3
H21E H 0.1750 0.4022 0.8553 0.162 Uiso 0.22 1 calc R U P A 3
H21F H 0.1934 0.3140 0.8754 0.162 Uiso 0.22 1 calc R U P A 3
C22A C 0.220(2) 0.2664(10) 0.7092(14) 0.057(5) Uiso 0.22 1 d D . P A 3
H22D H 0.1295 0.2530 0.6958 0.086 Uiso 0.22 1 calc R U P A 3
H22E H 0.2667 0.2308 0.7546 0.086 Uiso 0.22 1 calc R U P A 3
H22F H 0.2545 0.2643 0.6513 0.086 Uiso 0.22 1 calc R U P A 3
C23A C 0.1807(15) 0.3997(8) 0.6725(11) 0.086(5) Uiso 0.22 1 d D . P A 3
H23A H 0.1898 0.3762 0.6125 0.104 Uiso 0.22 1 calc R U P A 3
H23B H 0.0880 0.4033 0.6723 0.104 Uiso 0.22 1 calc R U P A 3
C24A C 0.2296(13) 0.4771(8) 0.6718(12) 0.083(6) Uiso 0.22 1 d D . P A 3
H24A H 0.1933 0.5064 0.7184 0.100 Uiso 0.22 1 calc R U P A 3
H24B H 0.1950 0.4990 0.6096 0.100 Uiso 0.22 1 calc R U P A 3
N22A N 0.3709(13) 0.4898(8) 0.6911(11) 0.023(3) Uiso 0.22 1 d D . P A 3
C25A C 0.4039(16) 0.5657(8) 0.7332(13) 0.066(5) Uiso 0.22 1 d D . P A 3
H25D H 0.3595 0.6045 0.6916 0.099 Uiso 0.22 1 calc R U P A 3
H25E H 0.4963 0.5735 0.7416 0.099 Uiso 0.22 1 calc R U P A 3
H25F H 0.3775 0.5686 0.7941 0.099 Uiso 0.22 1 calc R U P A 3
C26A C 0.420(4) 0.489(2) 0.601(2) 0.053(8) Uiso 0.22 1 d D . P A 3
H26D H 0.3827 0.5314 0.5621 0.079 Uiso 0.22 1 calc R U P A 3
H26E H 0.3960 0.4418 0.5683 0.079 Uiso 0.22 1 calc R U P A 3
H26F H 0.5131 0.4940 0.6147 0.079 Uiso 0.22 1 calc R U P A 3
N31 N 0.61132(15) 0.44129(8) 0.93618(11) 0.0406(4) Uani 1 1 d . . . . .
C31 C 0.7262(2) 0.46536(13) 0.89711(19) 0.0665(7) Uani 1 1 d . . . . .
H31A H 0.7856 0.4926 0.9453 0.100 Uiso 1 1 calc R U . . .
H31B H 0.6990 0.4983 0.8431 0.100 Uiso 1 1 calc R U . . .
H31C H 0.7687 0.4209 0.8776 0.100 Uiso 1 1 calc R U . . .
C32 C 0.6501(2) 0.37749(12) 1.00372(15) 0.0600(6) Uani 1 1 d . . . . .
H32A H 0.7006 0.3973 1.0619 0.090 Uiso 1 1 calc R U . . .
H32B H 0.7013 0.3412 0.9760 0.090 Uiso 1 1 calc R U . . .
H32C H 0.5736 0.3526 1.0171 0.090 Uiso 1 1 calc R U . . .
C33 C 0.56494(18) 0.50762(10) 0.98530(14) 0.0429(5) Uani 1 1 d . . . . .
H33A H 0.5564 0.5518 0.9432 0.052 Uiso 1 1 calc R U . . .
H33B H 0.6293 0.5199 1.0416 0.052 Uiso 1 1 calc R U . . .
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'
Na Na 0.0362 0.0249 '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'
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
C1 Na1 N21A 120.5(5) . .
C1 Na1 N21 121.77(14) . .
C1 Na1 N22 132.09(11) . .
N21 Na1 N22 72.86(13) . .
C1 Na1 N22A 136.8(3) . .
N21A Na1 N22A 73.8(4) . .
C1 Na1 N31 100.24(6) . .
N21A Na1 N31 127.5(5) . .
N21 Na1 N31 124.32(15) . .
N22 Na1 N31 106.11(10) . .
N22A Na1 N31 99.4(3) . .
Si12 C1 Si11 120.91(10) . .
Si12 C1 Na1 110.48(9) . .
Si11 C1 Na1 114.48(9) . .
C1 Si11 C112 112.80(10) . .
C1 Si11 C113 113.99(10) . .
C112 Si11 C113 105.78(11) . .
C1 Si11 C111 114.33(10) . .
C112 Si11 C111 105.37(11) . .
C113 Si11 C111 103.63(12) . .
C1 Si12 C122 111.11(10) . .
C1 Si12 C123 112.79(10) . .
C122 Si12 C123 107.17(11) . .
C1 Si12 C121 116.50(10) . .
C122 Si12 C121 103.97(10) . .
C123 Si12 C121 104.49(11) . .
C21 N21 C22 108.8(4) . .
C21 N21 C23 109.7(5) . .
C22 N21 C23 110.1(5) . .
C21 N21 Na1 118.8(4) . .
C22 N21 Na1 102.4(4) . .
C23 N21 Na1 106.8(3) . .
N21 C23 C24 112.6(3) . .
N22 C24 C23 112.8(3) . .
C26 N22 C24 110.2(5) . .
C26 N22 C25 107.3(5) . .
C24 N22 C25 109.9(3) . .
C26 N22 Na1 114.6(5) . .
C24 N22 Na1 105.8(2) . .
C25 N22 Na1 109.0(3) . .
C21A N21A C23A 109.1(17) . .
C21A N21A C22A 109.2(16) . .
C23A N21A C22A 107.9(17) . .
C21A N21A Na1 118.3(17) . .
C23A N21A Na1 105.9(12) . .
C22A N21A Na1 106.0(16) . .
C24A C23A N21A 120.9(14) . .
C23A C24A N22A 119.0(12) . .
C26A N22A C24A 109.8(17) . .
C26A N22A C25A 105.7(16) . .
C24A N22A C25A 111.3(12) . .
C26A N22A Na1 105.1(19) . .
C24A N22A Na1 107.1(9) . .
C25A N22A Na1 117.4(11) . .
C32 N31 C31 108.48(17) . .
C32 N31 C33 110.67(16) . .
C31 N31 C33 108.60(14) . .
C32 N31 Na1 102.77(12) . .
C31 N31 Na1 99.79(13) . .
C33 N31 Na1 125.26(12) . .
N31 C33 C33 112.57(18) . 3_667
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Na1 C1 2.5201(19) .
Na1 N21A 2.52(3) .
Na1 N21 2.561(8) .
Na1 N22 2.569(5) .
Na1 N22A 2.600(16) .
Na1 N31 2.6354(18) .
C1 Si12 1.808(2) .
C1 Si11 1.808(2) .
Si11 C112 1.891(2) .
Si11 C113 1.899(2) .
Si11 C111 1.902(2) .
Si12 C122 1.890(2) .
Si12 C123 1.899(2) .
Si12 C121 1.911(2) .
N21 C21 1.459(5) .
N21 C22 1.476(5) .
N21 C23 1.475(5) .
C23 C24 1.534(4) .
C24 N22 1.467(4) .
N22 C26 1.466(6) .
N22 C25 1.488(5) .
N21A C21A 1.471(16) .
N21A C23A 1.479(16) .
N21A C22A 1.487(15) .
C23A C24A 1.443(14) .
C24A N22A 1.467(14) .
N22A C26A 1.466(15) .
N22A C25A 1.465(13) .
N31 C32 1.476(3) .
N31 C31 1.476(3) .
N31 C33 1.479(2) .
C33 C33 1.517(4) 3_667
