#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/41/7014181.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_7014181
loop_
_publ_author_name
'Oakley, Sarah H.'
'Coles, Martyn P.'
'Hitchcock, Peter B.'
_publ_section_title
;
 Poly(guanidyl)silanes as a new class of chelating, N-based ligand.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1113
_journal_page_last               1114
_journal_paper_doi               10.1039/b402718c
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H39 N9 Si1'
_chemical_formula_sum            'C22 H39 N9 Si'
_chemical_formula_weight         457.71
_chemical_name_common            '[MeSi(C7H12N3)3]'
_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/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-04-16T09:21:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.074(1)
_cell_angle_beta                 91.011(1)
_cell_angle_gamma                94.329(1)
_cell_formula_units_Z            2
_cell_length_a                   8.3920(1)
_cell_length_b                   8.7131(1)
_cell_length_c                   16.3865(2)
_cell_measurement_reflns_used    13558
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1163.05(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.100119
_diffrn_orient_matrix_UB_12      -0.75922E-2
_diffrn_orient_matrix_UB_13      -0.323754E-1
_diffrn_orient_matrix_UB_21      0.651266E-1
_diffrn_orient_matrix_UB_22      0.39303E-1
_diffrn_orient_matrix_UB_23      0.533624E-1
_diffrn_orient_matrix_UB_31      0.58081E-2
_diffrn_orient_matrix_UB_32      -0.111235
_diffrn_orient_matrix_UB_33      0.58582E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21882
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.7
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.7553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                4809
_reflns_number_total             5235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402718c.txt
_cod_data_source_block           (2)-apr2203
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C22 H39 N9 Si1'
_cod_database_code               7014181
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
Si Si 0.17192(4) 0.10126(3) 0.254265(19) 0.01755(10) Uani 1 1 d . . .
N1 N 0.22581(13) 0.14136(11) 0.36189(6) 0.0208(2) Uani 1 1 d . . .
N2 N 0.19481(14) -0.12516(12) 0.35120(6) 0.0251(2) Uani 1 1 d . . .
N3 N 0.26063(14) 0.04296(13) 0.48413(6) 0.0260(2) Uani 1 1 d . . .
N4 N 0.16331(12) 0.28576(11) 0.22905(6) 0.0204(2) Uani 1 1 d . . .
N5 N -0.05281(13) 0.32291(12) 0.31086(7) 0.0248(2) Uani 1 1 d . . .
N6 N -0.01539(12) 0.47269(12) 0.20732(7) 0.0228(2) Uani 1 1 d . . .
N7 N 0.33825(12) 0.01667(12) 0.20434(6) 0.0199(2) Uani 1 1 d . . .
N8 N 0.20698(16) -0.01997(15) 0.07765(7) 0.0353(3) Uani 1 1 d . . .
N9 N 0.41889(14) -0.17822(13) 0.09026(7) 0.0276(2) Uani 1 1 d . . .
C1 C 0.22552(14) 0.01396(14) 0.39951(7) 0.0194(2) Uani 1 1 d . . .
C2 C 0.25010(16) 0.30201(14) 0.41495(8) 0.0249(3) Uani 1 1 d . . .
H2A H 0.1486 0.3333 0.4412 0.03 Uiso 1 1 calc R . .
H2B H 0.2832 0.3774 0.3802 0.03 Uiso 1 1 calc R . .
C3 C 0.37774(16) 0.30778(16) 0.48247(9) 0.0292(3) Uani 1 1 d . . .
H3A H 0.48 0.2787 0.4564 0.035 Uiso 1 1 calc R . .
H3B H 0.3948 0.4163 0.5179 0.035 Uiso 1 1 calc R . .
C4 C 0.32494(16) 0.19387(16) 0.53551(8) 0.0290(3) Uani 1 1 d . . .
H4A H 0.4172 0.1773 0.5701 0.035 Uiso 1 1 calc R . .
H4B H 0.2423 0.2399 0.5739 0.035 Uiso 1 1 calc R . .
C5 C 0.22472(19) -0.07857(17) 0.53097(8) 0.0325(3) Uani 1 1 d . . .
H5A H 0.1591 -0.0357 0.5792 0.039 Uiso 1 1 calc R . .
H5B H 0.3258 -0.1078 0.5532 0.039 Uiso 1 1 calc R . .
C6 C 0.13605(18) -0.22404(17) 0.47688(9) 0.0334(3) Uani 1 1 d . . .
H6A H 0.0213 -0.207 0.4721 0.04 Uiso 1 1 calc R . .
H6B H 0.1455 -0.3154 0.5028 0.04 Uiso 1 1 calc R . .
C7 C 0.20599(16) -0.25791(14) 0.39084(8) 0.0263(3) Uani 1 1 d . . .
H7A H 0.3196 -0.2792 0.3958 0.032 Uiso 1 1 calc R . .
H7B H 0.1479 -0.3535 0.3553 0.032 Uiso 1 1 calc R . .
C8 C 0.02668(14) 0.36404(13) 0.25163(7) 0.0193(2) Uani 1 1 d . . .
C9 C 0.28468(15) 0.35591(15) 0.18242(8) 0.0249(3) Uani 1 1 d . . .
H9A H 0.3591 0.2761 0.1583 0.03 Uiso 1 1 calc R . .
H9B H 0.3471 0.4451 0.2208 0.03 Uiso 1 1 calc R . .
C10 C 0.20568(16) 0.41440(16) 0.11288(9) 0.0288(3) Uani 1 1 d . . .
H10A H 0.1466 0.3249 0.0731 0.035 Uiso 1 1 calc R . .
H10B H 0.2877 0.4632 0.0818 0.035 Uiso 1 1 calc R . .
C11 C 0.09151(16) 0.53513(16) 0.15128(9) 0.0295(3) Uani 1 1 d . . .
H11A H 0.1532 0.6323 0.183 0.035 Uiso 1 1 calc R . .
H11B H 0.0277 0.5633 0.1062 0.035 Uiso 1 1 calc R . .
C12 C -0.14503(15) 0.56984(15) 0.23848(8) 0.0258(3) Uani 1 1 d . . .
H12A H -0.1907 0.6116 0.1926 0.031 Uiso 1 1 calc R . .
H12B H -0.1032 0.6607 0.2836 0.031 Uiso 1 1 calc R . .
C13 C -0.27415(15) 0.47222(15) 0.27213(8) 0.0265(3) Uani 1 1 d . . .
H13A H -0.3258 0.3895 0.2257 0.032 Uiso 1 1 calc R . .
H13B H -0.3569 0.5407 0.2983 0.032 Uiso 1 1 calc R . .
C14 C -0.19964(16) 0.39621(15) 0.33650(9) 0.0272(3) Uani 1 1 d . . .
H14A H -0.1767 0.4778 0.389 0.033 Uiso 1 1 calc R . .
H14B H -0.2785 0.3148 0.3489 0.033 Uiso 1 1 calc R . .
C15 C 0.31950(15) -0.06089(14) 0.12033(7) 0.0209(2) Uani 1 1 d . A .
C16 C 0.49071(15) 0.00786(15) 0.24717(8) 0.0239(2) Uani 1 1 d . A .
H16A H 0.4833 0.0517 0.3081 0.029 Uiso 1 1 calc R . .
H16B H 0.5764 0.0714 0.226 0.029 Uiso 1 1 calc R . .
C17 C 0.53072(16) -0.16270(16) 0.23175(8) 0.0272(3) Uani 1 1 d . . .
H17A H 0.6321 -0.1698 0.262 0.033 Uiso 1 1 calc R A .
H17B H 0.4449 -0.2269 0.2524 0.033 Uiso 1 1 calc R . .
C18 C 0.54686(16) -0.22380(15) 0.13855(9) 0.0285(3) Uani 1 1 d . A .
H18A H 0.651 -0.1817 0.1217 0.034 Uiso 1 1 calc R . .
H18B H 0.5454 -0.3405 0.1258 0.034 Uiso 1 1 calc R . .
C22 C -0.01922(15) -0.02082(14) 0.22344(8) 0.0250(3) Uani 1 1 d . . .
H22A H 0.0027 -0.1266 0.1922 0.038 Uiso 1 1 calc R . .
H22B H -0.0842 0.0288 0.188 0.038 Uiso 1 1 calc R . .
H22C H -0.0773 -0.0293 0.2738 0.038 Uiso 1 1 calc R . .
C19 C 0.4210(2) -0.24398(19) 0.00008(9) 0.0387(3) Uani 0.620(5) 1 d P A 1
H19A H 0.3809 -0.3569 -0.012 0.046 Uiso 0.620(5) 1 calc PR A 1
H19B H 0.5327 -0.2379 -0.0182 0.046 Uiso 0.620(5) 1 calc PR A 1
C20 C 0.3184(3) -0.1566(3) -0.05043(14) 0.0374(7) Uani 0.620(5) 1 d P A 1
H20A H 0.3801 -0.0597 -0.0581 0.045 Uiso 0.620(5) 1 calc PR A 1
H20B H 0.2906 -0.2252 -0.1066 0.045 Uiso 0.620(5) 1 calc PR A 1
C21 C 0.1746(2) -0.1149(3) -0.00738(10) 0.0527(5) Uani 0.620(5) 1 d P A 1
H21A H 0.1086 -0.2128 -0.0049 0.063 Uiso 0.620(5) 1 calc PR A 1
H21B H 0.1123 -0.055 -0.0396 0.063 Uiso 0.620(5) 1 calc PR A 1
C19A C 0.4210(2) -0.24398(19) 0.00008(9) 0.0387(3) Uani 0.380(5) 1 d P A 2
H19C H 0.4641 -0.3492 -0.0116 0.046 Uiso 0.380(5) 1 calc PR A 2
H19D H 0.4878 -0.1733 -0.0275 0.046 Uiso 0.380(5) 1 calc PR A 2
C20A C 0.2439(5) -0.2576(5) -0.0316(2) 0.0345(11) Uani 0.380(5) 1 d P A 2
H20C H 0.2386 -0.2917 -0.0935 0.041 Uiso 0.380(5) 1 calc PR A 2
H20D H 0.1825 -0.3393 -0.0091 0.041 Uiso 0.380(5) 1 calc PR A 2
C21A C 0.1746(2) -0.1149(3) -0.00738(10) 0.0527(5) Uani 0.380(5) 1 d P A 2
H21C H 0.0573 -0.1379 -0.0153 0.063 Uiso 0.380(5) 1 calc PR A 2
H21D H 0.2085 -0.0486 -0.0467 0.063 Uiso 0.380(5) 1 calc PR A 2
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'
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
N4 Si N7 106.67(5) . . ?
N4 Si N1 106.07(5) . . ?
N7 Si N1 104.20(5) . . ?
N4 Si C22 110.25(5) . . ?
N7 Si C22 113.77(5) . . ?
N1 Si C22 115.22(5) . . ?
C1 N1 C2 118.78(10) . . ?
C1 N1 Si 117.43(8) . . ?
C2 N1 Si 123.30(8) . . ?
C1 N2 C7 115.95(10) . . ?
C1 N3 C4 124.90(11) . . ?
C1 N3 C5 120.86(11) . . ?
C4 N3 C5 114.13(10) . . ?
C8 N4 C9 119.06(9) . . ?
C8 N4 Si 116.55(8) . . ?
C9 N4 Si 124.30(8) . . ?
C8 N5 C14 119.37(10) . . ?
C8 N6 C12 117.70(10) . . ?
C8 N6 C11 123.43(10) . . ?
C12 N6 C11 115.35(10) . . ?
C15 N7 C16 117.35(10) . . ?
C15 N7 Si 117.95(8) . . ?
C16 N7 Si 124.38(8) . . ?
C15 N8 C21 116.61(12) . . ?
C15 N9 C18 125.24(10) . . ?
C15 N9 C19 119.24(11) . . ?
C18 N9 C19 114.43(11) . . ?
N2 C1 N3 124.70(11) . . ?
N2 C1 N1 116.82(10) . . ?
N3 C1 N1 118.47(10) . . ?
N1 C2 C3 109.85(10) . . ?
C4 C3 C2 109.14(11) . . ?
N3 C4 C3 111.43(10) . . ?
N3 C5 C6 111.64(11) . . ?
C5 C6 C7 109.32(11) . . ?
N2 C7 C6 111.18(11) . . ?
N5 C8 N6 125.83(11) . . ?
N5 C8 N4 116.05(10) . . ?
N6 C8 N4 118.07(10) . . ?
N4 C9 C10 109.98(10) . . ?
C9 C10 C11 108.60(11) . . ?
N6 C11 C10 110.72(10) . . ?
N6 C12 C13 109.93(10) . . ?
C12 C13 C14 109.14(10) . . ?
N5 C14 C13 114.45(10) . . ?
N8 C15 N9 125.32(11) . . ?
N8 C15 N7 116.84(11) . . ?
N9 C15 N7 117.81(10) . . ?
N7 C16 C17 109.64(10) . . ?
C18 C17 C16 108.25(11) . . ?
N9 C18 C17 111.89(10) . . ?
N9 C19 C20 112.47(13) . . ?
C21 C20 C19 110.23(18) . . ?
C20 C21 N8 112.49(16) . . ?
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
Si N4 1.7542(10) . ?
Si N7 1.7560(10) . ?
Si N1 1.7624(10) . ?
Si C22 1.8521(13) . ?
N1 C1 1.3862(15) . ?
N1 C2 1.4686(14) . ?
N2 C1 1.2938(15) . ?
N2 C7 1.4570(15) . ?
N3 C1 1.3745(15) . ?
N3 C4 1.4508(16) . ?
N3 C5 1.4591(17) . ?
N4 C8 1.3912(15) . ?
N4 C9 1.4628(15) . ?
N5 C8 1.2883(16) . ?
N5 C14 1.4555(15) . ?
N6 C8 1.3786(15) . ?
N6 C12 1.4574(15) . ?
N6 C11 1.4578(16) . ?
N7 C15 1.3901(15) . ?
N7 C16 1.4638(15) . ?
N8 C15 1.2838(17) . ?
N8 C21 1.4599(18) . ?
N9 C15 1.3780(15) . ?
N9 C18 1.4539(17) . ?
N9 C19 1.4600(17) . ?
C2 C3 1.5162(19) . ?
C3 C4 1.508(2) . ?
C5 C6 1.507(2) . ?
C6 C7 1.512(2) . ?
C9 C10 1.5116(18) . ?
C10 C11 1.5148(18) . ?
C12 C13 1.5152(18) . ?
C13 C14 1.5157(18) . ?
C16 C17 1.5144(17) . ?
C17 C18 1.5114(19) . ?
C19 C20 1.538(3) . ?
C20 C21 1.438(3) . ?
