#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:51:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179767 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/63/7006331.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_7006331
loop_
_publ_author_name
'Avent, Anthony G.'
'Antolini, Floria'
'Hitchcock, Peter B.'
'Khvostov, Alexei V.'
'Lappert, Michael F.'
'Protchenko, Andrey V.'
_publ_section_title
;
 Reactions between a sodium amide Na[N(SiMe3)R1] (R1 = SiMe3, SiMe2Ph
 or But) and a cyanoalkane RCN (R = Ad or Bu(t)).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              919
_journal_page_last               927
_journal_paper_doi               10.1039/b506753g
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H58 N4 Na2 Si4'
_chemical_formula_sum            'C32 H58 N4 Na2 Si4'
_chemical_formula_weight         657.16
_chemical_name_common            ((Na(tBuCN)(Me3SiNSiMe2Ph))2)
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-02-04T15:51:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.666(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9961(3)
_cell_length_b                   10.9755(2)
_cell_length_c                   17.7283(5)
_cell_measurement_reflns_used    10080
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     2060.11(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19890
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.71
_exptl_absorpt_coefficient_mu    0.19
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0516P)²+0.5492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                4918
_reflns_number_total             5976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b506753g.txt
_cod_data_source_block           (2b)-feb1000
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7006331
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na -0.58873(5) -0.04140(5) 0.04897(3) 0.03199(13) Uani 1 1 d . . .
Si1 Si -0.26835(3) -0.03568(3) 0.135663(19) 0.02667(9) Uani 1 1 d . . .
Si2 Si -0.38351(3) -0.24866(3) 0.02993(2) 0.02846(9) Uani 1 1 d . . .
N1 N -0.37077(9) -0.10177(9) 0.05866(6) 0.0270(2) Uani 1 1 d . . .
N2 N -0.68111(14) -0.04567(14) 0.15627(8) 0.0487(3) Uani 1 1 d . . .
C1 C -0.34215(15) 0.01607(15) 0.21448(8) 0.0410(3) Uani 1 1 d . . .
H1A H -0.4168 0.0658 0.1911 0.061 Uiso 1 1 calc R . .
H1B H -0.2809 0.0646 0.2533 0.061 Uiso 1 1 calc R . .
H1C H -0.3671 -0.0552 0.2401 0.061 Uiso 1 1 calc R . .
C2 C -0.12765(14) -0.12825(14) 0.18990(9) 0.0429(3) Uani 1 1 d . . .
H2A H -0.083 -0.1589 0.1528 0.064 Uiso 1 1 calc R . .
H2B H -0.1562 -0.1971 0.2159 0.064 Uiso 1 1 calc R . .
H2C H -0.0705 -0.077 0.2292 0.064 Uiso 1 1 calc R . .
C3 C -0.19555(11) 0.10331(11) 0.10026(7) 0.0282(2) Uani 1 1 d . . .
C4 C -0.19161(14) 0.22034(12) 0.13186(8) 0.0366(3) Uani 1 1 d . . .
H4 H -0.2282 0.2342 0.1739 0.044 Uiso 1 1 calc R . .
C5 C -0.13528(16) 0.31737(13) 0.10323(10) 0.0452(3) Uani 1 1 d . . .
H5 H -0.1348 0.3962 0.1254 0.054 Uiso 1 1 calc R . .
C6 C -0.08036(15) 0.29932(15) 0.04288(9) 0.0462(4) Uani 1 1 d . . .
H6 H -0.0422 0.3655 0.0233 0.055 Uiso 1 1 calc R . .
C7 C -0.08109(14) 0.18470(15) 0.01100(9) 0.0420(3) Uani 1 1 d . . .
H7 H -0.0424 0.1715 -0.0302 0.05 Uiso 1 1 calc R . .
C8 C -0.13836(13) 0.08841(12) 0.03911(8) 0.0338(3) Uani 1 1 d . . .
H8 H -0.1388 0.0101 0.0162 0.041 Uiso 1 1 calc R . .
C9 C -0.23435(17) -0.34000(16) 0.04802(12) 0.0575(5) Uani 1 1 d . . .
H9A H -0.1912 -0.3397 0.1042 0.086 Uiso 1 1 calc R . .
H9B H -0.179 -0.304 0.019 0.086 Uiso 1 1 calc R . .
H9C H -0.2548 -0.424 0.0304 0.086 Uiso 1 1 calc R . .
C10 C -0.45459(18) -0.25887(16) -0.07874(10) 0.0525(4) Uani 1 1 d . . .
H10A H -0.5341 -0.2133 -0.0932 0.079 Uiso 1 1 calc R . .
H10B H -0.4709 -0.3444 -0.0939 0.079 Uiso 1 1 calc R . .
H10C H -0.3958 -0.2242 -0.1058 0.079 Uiso 1 1 calc R . .
C11 C -0.4922(3) -0.33666(18) 0.07525(16) 0.0814(8) Uani 1 1 d . . .
H11A H -0.5721 -0.2925 0.0673 0.122 Uiso 1 1 calc R . .
H11B H -0.4528 -0.3463 0.1315 0.122 Uiso 1 1 calc R . .
H11C H -0.5084 -0.4171 0.0506 0.122 Uiso 1 1 calc R . .
C12 C -0.70811(13) 0.00363(13) 0.20587(8) 0.0347(3) Uani 1 1 d . . .
C13 C -0.74129(12) 0.07204(13) 0.26933(8) 0.0327(3) Uani 1 1 d . . .
C14 C -0.76606(18) -0.01811(16) 0.32901(10) 0.0506(4) Uani 1 1 d . . .
H14A H -0.7882 0.0266 0.3713 0.076 Uiso 1 1 calc R . .
H14B H -0.69 -0.0668 0.3508 0.076 Uiso 1 1 calc R . .
H14C H -0.836 -0.072 0.3033 0.076 Uiso 1 1 calc R . .
C15 C -0.85975(16) 0.14761(17) 0.23265(11) 0.0528(4) Uani 1 1 d . . .
H15A H -0.8833 0.1944 0.2736 0.079 Uiso 1 1 calc R . .
H15B H -0.9293 0.0931 0.2071 0.079 Uiso 1 1 calc R . .
H15C H -0.8424 0.2037 0.1938 0.079 Uiso 1 1 calc R . .
C16 C -0.62981(17) 0.15611(19) 0.30611(12) 0.0606(5) Uani 1 1 d . . .
H16A H -0.6489 0.2035 0.3484 0.091 Uiso 1 1 calc R . .
H16B H -0.6154 0.2116 0.2661 0.091 Uiso 1 1 calc R . .
H16C H -0.5539 0.107 0.3274 0.091 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 0 '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
_geom_angle_publ_flag
N2 Na N1 127.89(5) . 3_455 ?
N2 Na N1 123.93(5) . . ?
N1 Na N1 101.50(3) 3_455 . ?
N1 Si1 C1 113.84(6) . . ?
N1 Si1 C2 117.36(6) . . ?
C1 Si1 C2 104.07(7) . . ?
N1 Si1 C3 109.06(5) . . ?
C1 Si1 C3 107.84(6) . . ?
C2 Si1 C3 103.87(6) . . ?
N1 Si2 C9 117.54(7) . . ?
N1 Si2 C10 110.18(7) . . ?
C9 Si2 C10 104.26(8) . . ?
N1 Si2 C11 111.93(7) . . ?
C9 Si2 C11 106.28(11) . . ?
C10 Si2 C11 105.77(11) . . ?
Si1 N1 Si2 129.85(6) . . ?
Si1 N1 Na 107.49(5) . 3_455 ?
Si2 N1 Na 113.62(5) . 3_455 ?
Si1 N1 Na 111.63(5) . . ?
Si2 N1 Na 103.76(5) . . ?
Na N1 Na 78.50(3) 3_455 . ?
C12 N2 Na 149.60(13) . . ?
C4 C3 C8 116.45(12) . . ?
C4 C3 Si1 125.03(10) . . ?
C8 C3 Si1 118.50(9) . . ?
C5 C4 C3 121.65(13) . . ?
C6 C5 C4 120.25(14) . . ?
C5 C6 C7 119.64(14) . . ?
C6 C7 C8 120.01(14) . . ?
C7 C8 C3 122.00(13) . . ?
C7 C8 Na 115.24(9) . 3_455 ?
C3 C8 Na 80.20(7) . 3_455 ?
N2 C12 C13 177.80(15) . . ?
C12 C13 C14 108.99(12) . . ?
C12 C13 C16 107.24(12) . . ?
C14 C13 C16 111.56(14) . . ?
C12 C13 C15 107.95(12) . . ?
C14 C13 C15 110.77(13) . . ?
C16 C13 C15 110.19(14) . . ?
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
Na N2 2.3867(14) . ?
Na N1 2.4185(11) 3_455 ?
Na N1 2.4475(11) . ?
Si1 N1 1.6816(11) . ?
Si1 C1 1.8831(14) . ?
Si1 C2 1.8833(14) . ?
Si1 C3 1.9061(13) . ?
Si2 N1 1.6851(11) . ?
Si2 C9 1.8746(16) . ?
Si2 C10 1.8766(17) . ?
Si2 C11 1.8776(18) . ?
N1 Na 2.4186(11) 3_455 ?
N2 C12 1.1380(18) . ?
C3 C4 1.3972(18) . ?
C3 C8 1.4019(18) . ?
C4 C5 1.395(2) . ?
C5 C6 1.378(2) . ?
C6 C7 1.378(2) . ?
C7 C8 1.3898(19) . ?
C8 Na 3.0298(14) 3_455 ?
C12 C13 1.4778(19) . ?
C13 C14 1.526(2) . ?
C13 C16 1.532(2) . ?
C13 C15 1.533(2) . ?
