#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:51:43 +0100 (vie 25 de mar de 2016) $
#$Revision: 179767 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/63/7006330.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_7006330
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         'C44 H70 N4 Na2 Si4'
_chemical_formula_sum            'C44 H70 N4 Na2 Si4'
_chemical_formula_weight         813.38
_chemical_name_common            ((Na(AdCN)(N(SiMe3)(SiMe2Ph)))2)
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-06-21T11:06:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                117.513(4)
_cell_angle_beta                 92.062(5)
_cell_angle_gamma                100.720(5)
_cell_formula_units_Z            1
_cell_length_a                   10.3261(7)
_cell_length_b                   11.1180(12)
_cell_length_c                   11.9940(10)
_cell_measurement_reflns_used    28349
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.638
_cell_measurement_wavelength     0.71073
_cell_volume                     1188.14(19)
_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 0.96
_diffrn_measured_fraction_theta_max 0.96
_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  0.0963
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13439
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.095
_refine_ls_R_factor_gt           0.0741
_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)+(0.0477P)²+1.6178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2046
_reflns_number_gt                4248
_reflns_number_total             5493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b506753g.txt
_cod_data_source_block           (2a)-jun2500
_cod_original_cell_volume        1188.14(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7006330
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
Na Na -0.09283(12) 0.88795(13) 0.02099(13) 0.0377(3) Uani 1 1 d . . .
Si1 Si 0.22485(9) 0.87713(9) 0.02666(8) 0.0331(2) Uani 1 1 d . . .
Si2 Si 0.08880(9) 0.79273(9) -0.23711(8) 0.0350(2) Uani 1 1 d . . .
N1 N 0.1087(3) 0.8738(3) -0.0774(2) 0.0323(6) Uani 1 1 d . . .
N2 N -0.2686(3) 0.6893(3) -0.0342(3) 0.0494(8) Uani 1 1 d . . .
C1 C 0.3257(4) 0.7413(4) -0.0362(4) 0.0479(9) Uani 1 1 d . . .
H1A H 0.2659 0.6488 -0.0827 0.072 Uiso 1 1 calc R . .
H1B H 0.381 0.7465 0.0347 0.072 Uiso 1 1 calc R . .
H1C H 0.383 0.7579 -0.0934 0.072 Uiso 1 1 calc R . .
C2 C 0.3527(3) 1.0469(4) 0.1120(4) 0.0447(8) Uani 1 1 d . . .
H2A H 0.3076 1.1241 0.1478 0.067 Uiso 1 1 calc R . .
H2B H 0.4095 1.0579 0.0522 0.067 Uiso 1 1 calc R . .
H2C H 0.4074 1.047 0.1806 0.067 Uiso 1 1 calc R . .
C3 C 0.1412(3) 0.8454(4) 0.1528(3) 0.0355(7) Uani 1 1 d . . .
C4 C 0.0409(3) 0.7256(4) 0.1158(4) 0.0433(8) Uani 1 1 d . . .
H4 H 0.0137 0.6629 0.028 0.052 Uiso 1 1 calc R . .
C5 C -0.0203(4) 0.6956(4) 0.2047(4) 0.0523(10) Uani 1 1 d . . .
H5 H -0.0883 0.6134 0.1768 0.063 Uiso 1 1 calc R . .
C6 C 0.0168(4) 0.7839(5) 0.3317(4) 0.0495(9) Uani 1 1 d . . .
H6 H -0.0246 0.7625 0.3918 0.059 Uiso 1 1 calc R . .
C7 C 0.1149(4) 0.9045(4) 0.3727(4) 0.0467(8) Uani 1 1 d . . .
H7 H 0.1404 0.9668 0.4608 0.056 Uiso 1 1 calc R . .
C8 C 0.1763(3) 0.9338(4) 0.2831(3) 0.0393(7) Uani 1 1 d . . .
H8 H 0.244 1.0164 0.3119 0.047 Uiso 1 1 calc R . .
C9 C 0.1696(5) 0.9115(5) -0.2997(4) 0.0671(12) Uani 1 1 d . . .
H9A H 0.1403 0.9992 -0.2594 0.101 Uiso 1 1 calc R . .
H9B H 0.1439 0.8664 -0.3918 0.101 Uiso 1 1 calc R . .
H9C H 0.2666 0.9306 -0.2804 0.101 Uiso 1 1 calc R . .
C10 C 0.1517(5) 0.6287(5) -0.3201(4) 0.0700(14) Uani 1 1 d . . .
H10A H 0.1116 0.5622 -0.292 0.105 Uiso 1 1 calc R . .
H10B H 0.2487 0.651 -0.2995 0.105 Uiso 1 1 calc R . .
H10C H 0.1274 0.5877 -0.4121 0.105 Uiso 1 1 calc R . .
C11 C -0.0921(4) 0.7383(5) -0.3047(4) 0.0543(10) Uani 1 1 d . . .
H11A H -0.14 0.6749 -0.2764 0.081 Uiso 1 1 calc R . .
H11B H -0.101 0.6908 -0.3977 0.081 Uiso 1 1 calc R . .
H11C H -0.1297 0.8208 -0.2754 0.081 Uiso 1 1 calc R . .
C12 C -0.3342(3) 0.5900(4) -0.1148(3) 0.0388(7) Uani 1 1 d . . .
C13 C -0.4159(3) 0.4640(3) -0.2222(3) 0.0342(7) Uani 1 1 d . . .
C14 C -0.5306(3) 0.3955(3) -0.1762(3) 0.0371(7) Uani 1 1 d . . .
H14A H -0.4939 0.3695 -0.1152 0.044 Uiso 1 1 calc R . .
H14B H -0.5868 0.462 -0.1328 0.044 Uiso 1 1 calc R . .
C15 C -0.6142(3) 0.2658(3) -0.2907(3) 0.0398(7) Uani 1 1 d . . .
H15 H -0.6883 0.2208 -0.2614 0.048 Uiso 1 1 calc R . .
C16 C -0.6723(3) 0.3068(4) -0.3832(3) 0.0441(8) Uani 1 1 d . . .
H16A H -0.7291 0.3728 -0.3407 0.053 Uiso 1 1 calc R . .
H16B H -0.728 0.2231 -0.4567 0.053 Uiso 1 1 calc R . .
C17 C -0.5589(4) 0.3748(4) -0.4288(4) 0.0499(9) Uani 1 1 d . . .
H17 H -0.5972 0.4009 -0.4901 0.06 Uiso 1 1 calc R . .
C18 C -0.4749(4) 0.5055(4) -0.3158(3) 0.0438(8) Uani 1 1 d . . .
H18A H -0.5308 0.5726 -0.2731 0.053 Uiso 1 1 calc R . .
H18B H -0.4023 0.5506 -0.3452 0.053 Uiso 1 1 calc R . .
C19 C -0.3277(3) 0.3601(4) -0.2884(4) 0.0448(8) Uani 1 1 d . . .
H19A H -0.253 0.4039 -0.3169 0.054 Uiso 1 1 calc R . .
H19B H -0.2903 0.3329 -0.2286 0.054 Uiso 1 1 calc R . .
C20 C -0.4138(4) 0.2321(4) -0.4023(4) 0.0549(10) Uani 1 1 d . . .
H20 H -0.3578 0.1643 -0.4466 0.066 Uiso 1 1 calc R . .
C21 C -0.5274(4) 0.1630(4) -0.3568(4) 0.0526(10) Uani 1 1 d . . .
H21A H -0.5817 0.0781 -0.4301 0.063 Uiso 1 1 calc R . .
H21B H -0.4901 0.1355 -0.2971 0.063 Uiso 1 1 calc R . .
C22 C -0.4721(4) 0.2728(5) -0.4946(4) 0.0636(12) Uani 1 1 d . . .
H22A H -0.526 0.1887 -0.569 0.076 Uiso 1 1 calc R . .
H22B H -0.3993 0.3164 -0.525 0.076 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 122.77(11) . . ?
N2 Na N1 128.43(11) . 2_575 ?
N1 Na N1 101.15(9) . 2_575 ?
N1 Si1 C1 117.36(15) . . ?
N1 Si1 C2 114.09(15) . . ?
C1 Si1 C2 104.30(18) . . ?
N1 Si1 C3 109.57(13) . . ?
C1 Si1 C3 103.41(16) . . ?
C2 Si1 C3 107.15(16) . . ?
N1 Si2 C11 111.09(16) . . ?
N1 Si2 C10 117.56(17) . . ?
C11 Si2 C10 104.3(2) . . ?
N1 Si2 C9 111.74(18) . . ?
C11 Si2 C9 105.3(2) . . ?
C10 Si2 C9 105.9(2) . . ?
Si1 N1 Si2 130.09(16) . . ?
Si1 N1 Na 105.75(12) . . ?
Si2 N1 Na 116.55(13) . . ?
Si1 N1 Na 109.89(13) . 2_575 ?
Si2 N1 Na 103.40(12) . 2_575 ?
Na N1 Na 78.85(9) . 2_575 ?
C12 N2 Na 145.9(3) . . ?
C8 C3 C4 116.5(3) . . ?
C8 C3 Si1 123.9(3) . . ?
C4 C3 Si1 119.5(3) . . ?
C5 C4 C3 121.7(4) . . ?
C6 C5 C4 120.4(4) . . ?
C5 C6 C7 119.9(3) . . ?
C6 C7 C8 119.4(4) . . ?
C3 C8 C7 122.1(3) . . ?
N2 C12 C13 177.7(4) . . ?
C12 C13 C18 108.4(3) . . ?
C12 C13 C14 110.6(3) . . ?
C18 C13 C14 109.2(3) . . ?
C12 C13 C19 109.2(3) . . ?
C18 C13 C19 110.0(3) . . ?
C14 C13 C19 109.5(3) . . ?
C15 C14 C13 109.0(3) . . ?
C16 C15 C21 109.6(3) . . ?
C16 C15 C14 109.6(3) . . ?
C21 C15 C14 109.7(3) . . ?
C15 C16 C17 109.4(3) . . ?
C22 C17 C18 109.6(3) . . ?
C22 C17 C16 109.7(3) . . ?
C18 C17 C16 109.7(3) . . ?
C17 C18 C13 108.8(3) . . ?
C20 C19 C13 108.2(3) . . ?
C22 C20 C19 110.5(4) . . ?
C22 C20 C21 109.4(3) . . ?
C19 C20 C21 109.6(3) . . ?
C15 C21 C20 109.2(3) . . ?
C20 C22 C17 109.6(3) . . ?
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 2.384(3) . ?
Na N1 2.423(3) . ?
Na N1 2.453(3) 2_575 ?
Si1 N1 1.683(3) . ?
Si1 C1 1.877(4) . ?
Si1 C2 1.882(4) . ?
Si1 C3 1.906(3) . ?
Si1 Na 3.4138(15) 2_575 ?
Si2 N1 1.683(3) . ?
Si2 C11 1.879(4) . ?
Si2 C10 1.883(4) . ?
Si2 C9 1.885(4) . ?
N1 Na 2.453(3) 2_575 ?
N2 C12 1.140(4) . ?
C3 C8 1.396(5) . ?
C3 C4 1.397(5) . ?
C4 C5 1.395(5) . ?
C5 C6 1.367(6) . ?
C6 C7 1.384(6) . ?
C7 C8 1.399(5) . ?
C12 C13 1.465(5) . ?
C13 C18 1.542(4) . ?
C13 C14 1.545(4) . ?
C13 C19 1.547(5) . ?
C14 C15 1.527(5) . ?
C15 C16 1.523(5) . ?
C15 C21 1.527(5) . ?
C16 C17 1.530(5) . ?
C17 C22 1.521(6) . ?
C17 C18 1.526(5) . ?
C19 C20 1.526(5) . ?
C20 C22 1.520(6) . ?
C20 C21 1.537(6) . ?
