#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:41:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178790 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/44/4104457.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_4104457
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         'C32 H42 N2 Ni O4 Si'
_chemical_formula_sum            'C32 H42 N2 Ni O4 Si'
_chemical_formula_weight         605.48
_chemical_name_common            HLSi(OH)-Ni(CO)3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.839(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8617(5)
_cell_length_b                   20.0470(8)
_cell_length_c                   9.7565(4)
_cell_measurement_reflns_used    2638
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8916
_cell_measurement_theta_min      3.0358
_cell_volume                     1597.36(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8739
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0483P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                1666
_reflns_number_total             2896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9026727_si_002.cif
_cod_data_source_block           m14
_cod_original_cell_volume        1597.36(13)
_cod_database_code               4104457
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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 0.43374(7) 0.2500 0.45854(6) 0.0298(2) Uani 1 2 d S
Si1 Si 0.52070(17) 0.2500 0.27142(14) 0.0373(4) Uani 1 2 d S
N1 N 0.4789(2) 0.18286(12) 0.1382(2) 0.0203(6) Uani 1 1 d .
C1 C 0.5143(4) 0.12769(15) -0.0730(3) 0.0337(8) Uani 1 1 d .
H1A H 0.6143 0.1024 -0.0182 0.051 Uiso 1 1 calc R
H1B H 0.5133 0.1409 -0.1701 0.051 Uiso 1 1 calc R
H1C H 0.4185 0.0998 -0.0874 0.051 Uiso 1 1 calc R
C2 C 0.5092(3) 0.18800(16) 0.0124(3) 0.0252(7) Uani 1 1 d .
C3 C 0.5325(5) 0.2500 -0.0394(4) 0.0283(11) Uani 1 2 d S
H3 H 0.5684 0.2500 -0.1193 0.043 Uiso 1 2 calc SR
C6 C 0.4300(3) 0.11795(15) 0.1746(3) 0.0224(7) Uani 1 1 d .
C7 C 0.5503(3) 0.07247(16) 0.2593(3) 0.0249(7) Uani 1 1 d .
C8 C 0.4975(4) 0.01235(16) 0.2967(3) 0.0320(8) Uani 1 1 d .
H8 H 0.5763 -0.0185 0.3579 0.048 Uiso 1 1 calc R
C9 C 0.3340(4) -0.00350(16) 0.2473(3) 0.0368(9) Uani 1 1 d .
H9 H 0.3007 -0.0453 0.2719 0.055 Uiso 1 1 calc R
C10 C 0.2188(4) 0.04181(17) 0.1615(3) 0.0338(8) Uani 1 1 d .
H10 H 0.1061 0.0304 0.1267 0.051 Uiso 1 1 calc R
C11 C 0.2629(4) 0.10369(16) 0.1247(3) 0.0275(8) Uani 1 1 d .
C12 C 0.7331(3) 0.08607(16) 0.3102(3) 0.0288(8) Uani 1 1 d .
H12 H 0.7480 0.1274 0.2596 0.043 Uiso 1 1 calc R
C13 C 0.8212(4) 0.02813(17) 0.2681(4) 0.0436(9) Uani 1 1 d .
H13A H 0.8120 -0.0124 0.3204 0.065 Uiso 1 1 calc R
H13B H 0.9371 0.0394 0.2967 0.065 Uiso 1 1 calc R
H13C H 0.7707 0.0206 0.1605 0.065 Uiso 1 1 calc R
C14 C 0.8124(4) 0.09729(19) 0.4793(3) 0.0450(10) Uani 1 1 d .
H14A H 0.7519 0.1319 0.5076 0.068 Uiso 1 1 calc R
H14B H 0.9263 0.1115 0.5071 0.068 Uiso 1 1 calc R
H14C H 0.8097 0.0556 0.5308 0.068 Uiso 1 1 calc R
C15 C 0.1326(4) 0.15195(17) 0.0315(3) 0.0348(8) Uani 1 1 d .
H15 H 0.1830 0.1974 0.0482 0.052 Uiso 1 1 calc R
C16 C -0.0149(4) 0.1550(2) 0.0728(4) 0.0704(13) Uani 1 1 d .
H16A H -0.0765 0.1132 0.0442 0.106 Uiso 1 1 calc R
H16C H -0.0852 0.1923 0.0206 0.106 Uiso 1 1 calc R
H16B H 0.0213 0.1615 0.1804 0.106 Uiso 1 1 calc R
C17 C 0.0760(5) 0.1370(2) -0.1333(4) 0.0783(15) Uani 1 1 d .
H17A H 0.1689 0.1408 -0.1636 0.118 Uiso 1 1 calc R
H17B H -0.0093 0.1688 -0.1899 0.118 Uiso 1 1 calc R
H17C H 0.0317 0.0916 -0.1529 0.118 Uiso 1 1 calc R
C31 C 0.6257(7) 0.2500 0.6132(5) 0.0399(13) Uani 1 2 d S
C32 C 0.3213(4) 0.1756(2) 0.4604(3) 0.0404(9) Uani 1 1 d .
O1 O 0.7499(4) 0.2500 0.7084(4) 0.0629(12) Uani 1 2 d S
O2 O 0.2534(3) 0.12918(14) 0.4700(3) 0.0658(8) Uani 1 1 d .
O4 O 0.7358(3) 0.2500 0.3270(3) 0.0499(9) Uani 1 2 d S
H40 H 0.7800 0.2641 0.4147 0.060 Uiso 0.50 1 calc PR
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'
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_1
_geom_angle_site_symmetry_3
C31 Ni1 C32 109.99(12) . .
C31 Ni1 C32 109.99(12) . 4_565
C32 Ni1 C32 112.1(2) . 4_565
C31 Ni1 Si1 99.94(14) . .
C32 Ni1 Si1 112.07(10) . .
C32 Ni1 Si1 112.07(10) 4_565 .
O4 Si1 N1 96.66(10) . .
O4 Si1 N1 96.66(10) . 4_565
N1 Si1 N1 96.30(15) . 4_565
O4 Si1 Ni1 114.92(12) . .
N1 Si1 Ni1 123.17(8) . .
N1 Si1 Ni1 123.17(8) 4_565 .
C2 N1 C6 118.0(2) . .
C2 N1 Si1 122.4(2) . .
C6 N1 Si1 119.10(16) . .
N1 C2 C3 120.4(3) . .
N1 C2 C1 120.5(3) . .
C3 C2 C1 119.1(3) . .
C2 C3 C2 127.3(4) . 4_565
C11 C6 C7 122.2(3) . .
C11 C6 N1 118.2(3) . .
C7 C6 N1 119.6(2) . .
C8 C7 C6 117.5(3) . .
C8 C7 C12 119.5(3) . .
C6 C7 C12 123.0(3) . .
C9 C8 C7 121.6(3) . .
C8 C9 C10 119.4(3) . .
C9 C10 C11 121.9(3) . .
C10 C11 C6 117.3(3) . .
C10 C11 C15 120.1(3) . .
C6 C11 C15 122.6(3) . .
C7 C12 C14 111.2(2) . .
C7 C12 C13 111.3(3) . .
C14 C12 C13 109.1(2) . .
C11 C15 C16 113.8(3) . .
C11 C15 C17 111.9(3) . .
C16 C15 C17 109.0(3) . .
O1 C31 Ni1 177.9(4) . .
O2 C32 Ni1 176.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 C31 1.782(5) .
Ni1 C32 1.798(4) .
Ni1 C32 1.798(4) 4_565
Ni1 Si1 2.2403(12) .
Si1 O4 1.768(3) .
Si1 N1 1.807(2) .
Si1 N1 1.807(2) 4_565
N1 C2 1.358(3) .
N1 C6 1.459(3) .
C1 C2 1.479(4) .
C2 C3 1.387(3) .
C3 C2 1.387(3) 4_565
C6 C11 1.397(4) .
C6 C7 1.403(4) .
C7 C8 1.392(4) .
C7 C12 1.523(4) .
C8 C9 1.375(4) .
C9 C10 1.380(4) .
C10 C11 1.389(4) .
C11 C15 1.510(4) .
C12 C14 1.538(4) .
C12 C13 1.542(4) .
C15 C16 1.512(4) .
C15 C17 1.517(4) .
C31 O1 1.132(5) .
C32 O2 1.132(4) .
