#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:41:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178790 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/44/4104458.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_4104458
loop_
_publ_author_name
'Antje Meltzer'
'Carsten Präsang'
'Matthias Driess'
_publ_contact_author_address
;Technische Universität Berlin,
Institute of Chemistry
Strasse des 17. Juni 136, D-10623 Berlin, Germany
;
_publ_contact_author_email       matthias.driess@tu-berlin.de
_publ_contact_author_fax         +49(0)30-314-29732
_publ_contact_author_name        'Matthias Driess'
_publ_contact_author_phone       +49(0)30-314-29731
_publ_section_title
;
 Diketiminate Silicon(II) and Related NHSi Ligands Generated in the
 Coordination Sphere of Nickel(0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7232
_journal_page_last               7233
_journal_paper_doi               10.1021/ja9026727
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C36 H48 F3 N2 Ni O6 S Si'
_chemical_formula_sum            'C36 H48 F3 N2 Ni O6 S Si'
_chemical_formula_weight         780.62
_chemical_name_common            HLSi(OTf)-Ni(CO)3*1/2hexane
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_cell_angle_alpha                105.188(3)
_cell_angle_beta                 98.328(2)
_cell_angle_gamma                107.146(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8132(3)
_cell_length_b                   11.6057(3)
_cell_length_c                   17.4222(5)
_cell_measurement_reflns_used    8682
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.8500
_cell_measurement_theta_min      3.0595
_cell_volume                     1956.91(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14196
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0364
_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)+(0.0464P)²+0.2079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                5545
_reflns_number_total             6854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9026727_si_003.cif
_cod_data_source_block           m17
_cod_original_cell_volume        1956.91(9)
_cod_database_code               4104458
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
Ni1 Ni 0.08759(3) 0.33035(3) 0.401129(16) 0.02007(9) Uani 1 1 d .
Si1 Si 0.09609(6) 0.22620(5) 0.27832(3) 0.01495(13) Uani 1 1 d .
N1 N 0.19802(16) 0.29843(15) 0.21791(10) 0.0156(4) Uani 1 1 d .
N2 N 0.12459(17) 0.07657(15) 0.25345(10) 0.0161(4) Uani 1 1 d .
C1 C 0.2706(3) 0.2884(2) 0.08949(14) 0.0328(6) Uani 1 1 d .
H1A H 0.2309 0.3517 0.0821 0.049 Uiso 1 1 calc R
H1B H 0.2535 0.2234 0.0364 0.049 Uiso 1 1 calc R
H1C H 0.3670 0.3303 0.1121 0.049 Uiso 1 1 calc R
C2 C 0.2101(2) 0.22688(19) 0.14709(13) 0.0193(5) Uani 1 1 d .
C3 C 0.1679(2) 0.09407(19) 0.12543(13) 0.0201(5) Uani 1 1 d .
H3 H 0.1597 0.0481 0.0700 0.024 Uiso 1 1 calc R
C4 C 0.1368(2) 0.02337(19) 0.17750(13) 0.0185(5) Uani 1 1 d .
C5 C 0.1175(3) -0.1161(2) 0.14726(14) 0.0282(6) Uani 1 1 d .
H5A H 0.1868 -0.1328 0.1809 0.042 Uiso 1 1 calc R
H5B H 0.1238 -0.1401 0.0901 0.042 Uiso 1 1 calc R
H5C H 0.0295 -0.1661 0.1511 0.042 Uiso 1 1 calc R
C6 C 0.2639(2) 0.43736(19) 0.24449(13) 0.0182(5) Uani 1 1 d .
C7 C 0.3992(2) 0.4896(2) 0.28521(13) 0.0211(5) Uani 1 1 d .
C8 C 0.4607(2) 0.6220(2) 0.31181(15) 0.0299(6) Uani 1 1 d .
H8 H 0.5524 0.6595 0.3395 0.036 Uiso 1 1 calc R
C9 C 0.3901(3) 0.6989(2) 0.29836(16) 0.0339(6) Uani 1 1 d .
H9 H 0.4329 0.7888 0.3173 0.041 Uiso 1 1 calc R
C10 C 0.2575(2) 0.6458(2) 0.25748(15) 0.0302(6) Uani 1 1 d .
H10 H 0.2101 0.7001 0.2487 0.036 Uiso 1 1 calc R
C11 C 0.1913(2) 0.5145(2) 0.22869(13) 0.0224(5) Uani 1 1 d .
C12 C 0.4822(2) 0.4112(2) 0.30426(14) 0.0248(5) Uani 1 1 d .
H12 H 0.4264 0.3190 0.2784 0.030 Uiso 1 1 calc R
C13 C 0.6068(3) 0.4369(3) 0.27029(19) 0.0472(7) Uani 1 1 d .
H13A H 0.5806 0.4215 0.2112 0.071 Uiso 1 1 calc R
H13B H 0.6541 0.3801 0.2803 0.071 Uiso 1 1 calc R
H13C H 0.6655 0.5257 0.2976 0.071 Uiso 1 1 calc R
C14 C 0.5231(3) 0.4391(2) 0.39698(16) 0.0377(6) Uani 1 1 d .
H14A H 0.5767 0.5296 0.4234 0.057 Uiso 1 1 calc R
H14B H 0.5758 0.3873 0.4086 0.057 Uiso 1 1 calc R
H14C H 0.4431 0.4184 0.4182 0.057 Uiso 1 1 calc R
C15 C 0.0467(2) 0.4624(2) 0.18210(15) 0.0272(5) Uani 1 1 d .
H15 H 0.0161 0.3674 0.1663 0.033 Uiso 1 1 calc R
C16 C 0.0303(3) 0.4972(3) 0.10316(16) 0.0428(7) Uani 1 1 d .
H16A H 0.0570 0.5899 0.1169 0.064 Uiso 1 1 calc R
H16B H -0.0632 0.4573 0.0724 0.064 Uiso 1 1 calc R
H16C H 0.0866 0.4665 0.0696 0.064 Uiso 1 1 calc R
C17 C -0.0428(3) 0.5073(3) 0.23416(17) 0.0451(7) Uani 1 1 d .
H17A H -0.0370 0.4790 0.2824 0.068 Uiso 1 1 calc R
H17B H -0.1353 0.4712 0.2017 0.068 Uiso 1 1 calc R
H17C H -0.0136 0.6005 0.2518 0.068 Uiso 1 1 calc R
C18 C 0.1214(2) 0.00309(19) 0.31087(13) 0.0182(5) Uani 1 1 d .
C19 C 0.0000(2) -0.0747(2) 0.31754(14) 0.0236(5) Uani 1 1 d .
C20 C 0.0035(2) -0.1511(2) 0.36723(14) 0.0293(6) Uani 1 1 d .
H20 H -0.0780 -0.2054 0.3721 0.035 Uiso 1 1 calc R
C21 C 0.1212(3) -0.1496(2) 0.40898(15) 0.0333(6) Uani 1 1 d .
H21 H 0.1213 -0.2043 0.4411 0.040 Uiso 1 1 calc R
C22 C 0.2400(2) -0.0684(2) 0.40441(14) 0.0286(5) Uani 1 1 d .
H22 H 0.3214 -0.0666 0.4347 0.034 Uiso 1 1 calc R
C23 C 0.2439(2) 0.01092(19) 0.35659(13) 0.0213(5) Uani 1 1 d .
C24 C -0.1361(2) -0.0808(2) 0.27572(15) 0.0317(6) Uani 1 1 d .
H24 H -0.1219 -0.0198 0.2438 0.038 Uiso 1 1 calc R
C25 C -0.2107(3) -0.0373(3) 0.34009(18) 0.0445(7) Uani 1 1 d .
H25A H -0.2344 -0.1004 0.3684 0.067 Uiso 1 1 calc R
H25B H -0.2921 -0.0290 0.3129 0.067 Uiso 1 1 calc R
H25C H -0.1533 0.0452 0.3799 0.067 Uiso 1 1 calc R
C26 C -0.2208(3) -0.2124(3) 0.21595(18) 0.0480(7) Uani 1 1 d .
H26A H -0.1742 -0.2372 0.1737 0.072 Uiso 1 1 calc R
H26B H -0.3066 -0.2104 0.1901 0.072 Uiso 1 1 calc R
H26C H -0.2362 -0.2744 0.2456 0.072 Uiso 1 1 calc R
C27 C 0.3769(2) 0.1059(2) 0.35842(15) 0.0282(5) Uani 1 1 d .
H27 H 0.3610 0.1856 0.3560 0.034 Uiso 1 1 calc R
C28 C 0.4358(3) 0.0619(3) 0.28566(17) 0.0392(6) Uani 1 1 d .
H28A H 0.4445 -0.0207 0.2829 0.059 Uiso 1 1 calc R
H28B H 0.5239 0.1246 0.2930 0.059 Uiso 1 1 calc R
H28C H 0.3767 0.0537 0.2347 0.059 Uiso 1 1 calc R
C29 C 0.4820(3) 0.1413(3) 0.43798(18) 0.0476(7) Uani 1 1 d .
H29A H 0.5082 0.0678 0.4393 0.071 Uiso 1 1 calc R
H29B H 0.4445 0.1663 0.4850 0.071 Uiso 1 1 calc R
H29C H 0.5603 0.2126 0.4405 0.071 Uiso 1 1 calc R
C30 C 0.1807(2) 0.4973(2) 0.42478(14) 0.0277(5) Uani 1 1 d .
O1 O 0.23781(19) 0.60322(16) 0.44040(11) 0.0427(5) Uani 1 1 d .
C31 C -0.0864(3) 0.3055(2) 0.39111(15) 0.0327(6) Uani 1 1 d .
O2 O -0.19763(19) 0.2887(2) 0.37972(13) 0.0545(6) Uani 1 1 d .
C32 C 0.1604(2) 0.2672(2) 0.47153(14) 0.0271(5) Uani 1 1 d .
O3 O 0.21228(19) 0.22928(18) 0.51584(11) 0.0425(5) Uani 1 1 d .
O4 O -0.06221(14) 0.17085(13) 0.20237(8) 0.0188(3) Uani 1 1 d .
O5 O -0.10019(18) 0.16269(15) 0.05927(9) 0.0349(4) Uani 1 1 d .
O6 O -0.15351(16) -0.03509(14) 0.09359(10) 0.0314(4) Uani 1 1 d .
S1 S -0.13788(6) 0.09637(5) 0.11505(3) 0.02313(14) Uani 1 1 d .
C33 C -0.3015(3) 0.1019(3) 0.12453(17) 0.0421(7) Uani 1 1 d .
F1 F -0.34322(16) 0.04894(19) 0.17869(11) 0.0645(5) Uani 1 1 d .
F2 F -0.29964(17) 0.22050(17) 0.14671(12) 0.0688(5) Uani 1 1 d .
F3 F -0.38697(16) 0.03959(19) 0.05303(11) 0.0736(6) Uani 1 1 d .
C1S C -0.3664(4) 0.2885(3) -0.0533(2) 0.0682(10) Uani 1 1 d .
H1S1 H -0.4450 0.2155 -0.0586 0.102 Uiso 1 1 calc R
H1S2 H -0.2857 0.2749 -0.0304 0.102 Uiso 1 1 calc R
H1S3 H -0.3631 0.2976 -0.1074 0.102 Uiso 1 1 calc R
C2S C -0.3750(3) 0.4094(3) 0.00347(19) 0.0534(8) Uani 1 1 d .
H2S1 H -0.3783 0.3994 0.0579 0.064 Uiso 1 1 calc R
H2S2 H -0.2932 0.4819 0.0106 0.064 Uiso 1 1 calc R
C3S C -0.4942(3) 0.4403(2) -0.02749(16) 0.0423(7) Uani 1 1 d .
H3S1 H -0.5757 0.3673 -0.0348 0.051 Uiso 1 1 calc R
H3S2 H -0.4907 0.4498 -0.0820 0.051 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 '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_3
C32 Ni1 C31 116.11(11) .
C32 Ni1 C30 110.44(10) .
C31 Ni1 C30 110.04(11) .
C32 Ni1 Si1 107.21(7) .
C31 Ni1 Si1 103.39(8) .
C30 Ni1 Si1 109.22(7) .
N2 Si1 N1 97.73(8) .
N2 Si1 O4 96.61(7) .
N1 Si1 O4 95.84(7) .
N2 Si1 Ni1 123.77(6) .
N1 Si1 Ni1 123.66(6) .
O4 Si1 Ni1 112.97(5) .
C2 N1 C6 119.29(16) .
C2 N1 Si1 120.75(14) .
C6 N1 Si1 119.91(13) .
C4 N2 C18 118.06(16) .
C4 N2 Si1 119.66(13) .
C18 N2 Si1 121.99(13) .
N1 C2 C3 121.40(18) .
N1 C2 C1 120.28(18) .
C3 C2 C1 118.33(19) .
C4 C3 C2 125.96(19) .
N2 C4 C3 121.82(18) .
N2 C4 C5 120.10(18) .
C3 C4 C5 118.08(19) .
C7 C6 C11 121.58(19) .
C7 C6 N1 118.44(18) .
C11 C6 N1 119.97(19) .
C8 C7 C6 118.18(19) .
C8 C7 C12 117.9(2) .
C6 C7 C12 123.86(19) .
C9 C8 C7 120.9(2) .
C8 C9 C10 120.1(2) .
C9 C10 C11 121.6(2) .
C10 C11 C6 117.6(2) .
C10 C11 C15 118.86(19) .
C6 C11 C15 123.57(19) .
C7 C12 C13 111.99(19) .
C7 C12 C14 110.08(19) .
C13 C12 C14 109.6(2) .
C11 C15 C17 112.3(2) .
C11 C15 C16 111.25(19) .
C17 C15 C16 110.0(2) .
C19 C18 C23 121.44(19) .
C19 C18 N2 120.52(19) .
C23 C18 N2 118.01(18) .
C20 C19 C18 117.9(2) .
C20 C19 C24 117.3(2) .
C18 C19 C24 124.76(19) .
C21 C20 C19 121.5(2) .
C20 C21 C22 119.8(2) .
C21 C22 C23 121.8(2) .
C22 C23 C18 117.4(2) .
C22 C23 C27 119.8(2) .
C18 C23 C27 122.73(19) .
C19 C24 C26 113.0(2) .
C19 C24 C25 110.2(2) .
C26 C24 C25 110.3(2) .
C23 C27 C29 112.4(2) .
C23 C27 C28 114.1(2) .
C29 C27 C28 108.5(2) .
O1 C30 Ni1 178.8(2) .
O2 C31 Ni1 175.8(2) .
O3 C32 Ni1 176.9(2) .
S1 O4 Si1 146.26(10) .
O5 S1 O6 118.70(10) .
O5 S1 O4 112.82(9) .
O6 S1 O4 113.10(9) .
O5 S1 C33 106.01(12) .
O6 S1 C33 105.07(12) .
O4 S1 C33 98.37(11) .
F3 C33 F1 108.7(2) .
F3 C33 F2 108.1(2) .
F1 C33 F2 108.8(2) .
F3 C33 S1 109.0(2) .
F1 C33 S1 111.15(19) .
F2 C33 S1 111.13(19) .
C3S C2S C1S 113.5(3) .
C2S C3S C3S 114.9(3) 2_465
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 C32 1.787(2) .
Ni1 C31 1.792(3) .
Ni1 C30 1.803(3) .
Ni1 Si1 2.1942(6) .
Si1 N2 1.8051(17) .
Si1 N1 1.8108(17) .
Si1 O4 1.8286(15) .
N1 C2 1.343(3) .
N1 C6 1.469(2) .
N2 C4 1.349(3) .
N2 C18 1.473(2) .
C1 C2 1.495(3) .
C2 C3 1.399(3) .
C3 C4 1.387(3) .
C4 C5 1.504(3) .
C6 C7 1.402(3) .
C6 C11 1.405(3) .
C7 C8 1.398(3) .
C7 C12 1.515(3) .
C8 C9 1.376(3) .
C9 C10 1.376(3) .
C10 C11 1.393(3) .
C11 C15 1.512(3) .
C12 C13 1.530(3) .
C12 C14 1.531(3) .
C15 C17 1.528(3) .
C15 C16 1.532(3) .
C18 C19 1.397(3) .
C18 C23 1.408(3) .
C19 C20 1.397(3) .
C19 C24 1.517(3) .
C20 C21 1.365(3) .
C21 C22 1.378(3) .
C22 C23 1.390(3) .
C23 C27 1.523(3) .
C24 C26 1.524(3) .
C24 C25 1.540(4) .
C27 C29 1.533(3) .
C27 C28 1.536(3) .
C30 O1 1.138(3) .
C31 O2 1.138(3) .
C32 O3 1.141(3) .
O4 S1 1.5048(15) .
O5 S1 1.4230(16) .
O6 S1 1.4236(16) .
S1 C33 1.819(3) .
C33 F3 1.315(3) .
C33 F1 1.317(3) .
C33 F2 1.321(3) .
C1S C2S 1.527(4) .
C2S C3S 1.500(4) .
C3S C3S 1.516(5) 2_465
