#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:29:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180013 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/07/7030799.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_7030799
loop_
_publ_author_name
'Schmidt, David'
'Zell, Thomas'
'Schaub, Thomas'
'Radius, Udo'
_publ_section_title
;
 Si-H bond activation at {(NHC)2Ni(0)} leading to hydrido silyl and
 bis(silyl) complexes: a versatile tool for catalytic Si-H/D exchange,
 acceptorless dehydrogenative coupling of hydrosilanes, and hydrogenation
 of disilanes to hydrosilanes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10816
_journal_page_last               10827
_journal_paper_doi               10.1039/c4dt01250j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         C30H62N4NiO6Si2
_chemical_formula_sum            'C30 H62 N4 Ni O6 Si2'
_chemical_formula_weight         689.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           'SHELXL-97 + manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.576(2)
_cell_length_b                   12.144(2)
_cell_length_c                   14.883(3)
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.3335
_cell_measurement_theta_min      2.7335
_cell_volume                     1866.3(6)
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_collection       'Smart-NT v. 5.63'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7173
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0426
_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)+(0.0758P)²+0.1791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                3102
_reflns_number_total             3736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01250j2.cif
_cod_data_source_block           compound_trans_12
_cod_depositor_comments
'Adding full bibliography for 7030793--7030800.cif.'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7030799
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
Ni Ni 0.0000 0.5000 0.0000 0.02063(16) Uani 1 2 d S
N2 N -0.05177(19) 0.70833(15) 0.08083(13) 0.0252(4) Uani 1 1 d .
Si Si -0.09101(7) 0.41401(5) 0.10673(5) 0.0278(2) Uani 1 1 d .
O1 O -0.24232(18) 0.45868(17) 0.09845(13) 0.0408(5) Uani 1 1 d .
N1 N 0.14763(19) 0.66031(15) 0.12640(13) 0.0250(4) Uani 1 1 d .
O3 O -0.02414(19) 0.42066(15) 0.21944(12) 0.0396(5) Uani 1 1 d .
C1 C 0.0330(2) 0.62665(18) 0.07239(15) 0.0226(5) Uani 1 1 d .
C4 C 0.2683(2) 0.5979(2) 0.13585(17) 0.0292(5) Uani 1 1 d .
H4A H 0.2571 0.5447 0.0834 0.035 Uiso 1 1 calc R
C2 C 0.1339(3) 0.7610(2) 0.16632(18) 0.0332(6) Uani 1 1 d .
H2A H 0.2000 0.8011 0.2064 0.040 Uiso 1 1 calc R
O2 O -0.0991(2) 0.27885(15) 0.09111(15) 0.0507(6) Uani 1 1 d .
C3 C 0.0104(3) 0.7913(2) 0.13808(18) 0.0348(6) Uani 1 1 d .
H3A H -0.0278 0.8572 0.1541 0.042 Uiso 1 1 calc R
C6 C 0.3791(3) 0.6744(3) 0.1291(2) 0.0506(8) Uani 1 1 d .
H6A H 0.3553 0.7187 0.0729 0.076 Uiso 1 1 calc R
H6B H 0.4565 0.6308 0.1271 0.076 Uiso 1 1 calc R
H6C H 0.3972 0.7232 0.1828 0.076 Uiso 1 1 calc R
C5 C -0.1869(2) 0.7105(2) 0.03035(17) 0.0307(6) Uani 1 1 d .
H5A H -0.2105 0.6342 0.0075 0.037 Uiso 1 1 calc R
C15 C -0.0280(3) 0.5159(2) 0.27349(19) 0.0412(7) Uani 1 1 d .
H15A H -0.1186 0.5417 0.2654 0.049 Uiso 1 1 calc R
H15B H 0.0233 0.5753 0.2530 0.049 Uiso 1 1 calc R
C9 C -0.2764(3) 0.7425(3) 0.0925(2) 0.0489(8) Uani 1 1 d .
H9A H -0.2605 0.6946 0.1468 0.073 Uiso 1 1 calc R
H9B H -0.3665 0.7344 0.0591 0.073 Uiso 1 1 calc R
H9C H -0.2603 0.8193 0.1119 0.073 Uiso 1 1 calc R
C13 C -0.1453(4) 0.1965(2) 0.1401(2) 0.0553(8) Uani 1 1 d .
H13A H -0.2330 0.2167 0.1478 0.066 Uiso 1 1 calc R
H13B H -0.0883 0.1909 0.2022 0.066 Uiso 1 1 calc R
C11 C -0.3254(3) 0.4302(3) 0.1592(2) 0.0444(7) Uani 1 1 d .
H11A H -0.3500 0.4978 0.1884 0.053 Uiso 1 1 calc R
H11B H -0.2781 0.3814 0.2085 0.053 Uiso 1 1 calc R
C7 C 0.2947(3) 0.5322(3) 0.2240(2) 0.0518(8) Uani 1 1 d .
H7A H 0.2220 0.4822 0.2243 0.078 Uiso 1 1 calc R
H7B H 0.3049 0.5825 0.2766 0.078 Uiso 1 1 calc R
H7C H 0.3742 0.4893 0.2284 0.078 Uiso 1 1 calc R
C8 C -0.2019(3) 0.7857(3) -0.0534(2) 0.0499(8) Uani 1 1 d .
H8A H -0.1402 0.7637 -0.0906 0.075 Uiso 1 1 calc R
H8B H -0.1848 0.8620 -0.0329 0.075 Uiso 1 1 calc R
H8C H -0.2903 0.7798 -0.0904 0.075 Uiso 1 1 calc R
C16 C 0.0258(4) 0.4907(3) 0.3729(2) 0.0620(11) Uani 1 1 d .
H16A H 0.0218 0.5569 0.4099 0.093 Uiso 1 1 calc R
H16B H 0.1161 0.4669 0.3810 0.093 Uiso 1 1 calc R
H16C H -0.0251 0.4319 0.3930 0.093 Uiso 1 1 calc R
C12 C -0.4455(3) 0.3728(3) 0.1086(2) 0.0590(9) Uani 1 1 d .
H12A H -0.5010 0.3555 0.1516 0.088 Uiso 1 1 calc R
H12B H -0.4215 0.3045 0.0814 0.088 Uiso 1 1 calc R
H12C H -0.4924 0.4210 0.0598 0.088 Uiso 1 1 calc R
C14 C -0.1510(4) 0.0904(3) 0.0950(3) 0.0708(11) Uani 1 1 d .
H14A H -0.1928 0.0369 0.1284 0.106 Uiso 1 1 calc R
H14B H -0.0631 0.0656 0.0944 0.106 Uiso 1 1 calc R
H14C H -0.2011 0.0970 0.0317 0.106 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'
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'
O O 0.0106 0.0060 '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
C1 Ni C1 180.0 . 3_565
C1 Ni Si 88.30(7) . 3_565
C1 Ni Si 91.70(7) 3_565 3_565
C1 Ni Si 91.70(7) . .
C1 Ni Si 88.30(7) 3_565 .
Si Ni Si 180.00(3) 3_565 .
C1 N2 C3 110.6(2) . .
C1 N2 C5 123.72(19) . .
C3 N2 C5 125.6(2) . .
O2 Si O1 106.98(11) . .
O2 Si O3 100.71(11) . .
O1 Si O3 104.40(10) . .
O2 Si Ni 111.87(7) . .
O1 Si Ni 110.01(7) . .
O3 Si Ni 121.66(8) . .
C11 O1 Si 125.73(19) . .
C1 N1 C2 110.8(2) . .
C1 N1 C4 123.11(19) . .
C2 N1 C4 126.0(2) . .
C15 O3 Si 123.43(17) . .
N2 C1 N1 104.27(18) . .
N2 C1 Ni 127.51(17) . .
N1 C1 Ni 128.19(17) . .
N1 C4 C7 110.5(2) . .
N1 C4 C6 110.3(2) . .
C7 C4 C6 112.4(2) . .
N1 C4 H4A 107.8 . .
C7 C4 H4A 107.8 . .
C6 C4 H4A 107.8 . .
C3 C2 N1 107.2(2) . .
C3 C2 H2A 126.4 . .
N1 C2 H2A 126.4 . .
C13 O2 Si 130.8(2) . .
C2 C3 N2 107.1(2) . .
C2 C3 H3A 126.4 . .
N2 C3 H3A 126.4 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C5 C9 111.2(2) . .
N2 C5 C8 110.3(2) . .
C9 C5 C8 112.2(2) . .
N2 C5 H5A 107.6 . .
C9 C5 H5A 107.6 . .
C8 C5 H5A 107.6 . .
O3 C15 C16 110.1(3) . .
O3 C15 H15A 109.6 . .
C16 C15 H15A 109.6 . .
O3 C15 H15B 109.6 . .
C16 C15 H15B 109.6 . .
H15A C15 H15B 108.2 . .
C5 C9 H9A 109.5 . .
C5 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C5 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O2 C13 C14 112.4(3) . .
O2 C13 H13A 109.1 . .
C14 C13 H13A 109.1 . .
O2 C13 H13B 109.1 . .
C14 C13 H13B 109.1 . .
H13A C13 H13B 107.8 . .
O1 C11 C12 111.3(2) . .
O1 C11 H11A 109.4 . .
C12 C11 H11A 109.4 . .
O1 C11 H11B 109.4 . .
C12 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni C1 1.867(2) .
Ni C1 1.867(2) 3_565
Ni Si 2.2806(8) 3_565
Ni Si 2.2806(8) .
N2 C1 1.361(3) .
N2 C3 1.389(3) .
N2 C5 1.464(3) .
Si O2 1.657(2) .
Si O1 1.669(2) .
Si O3 1.6755(19) .
O1 C11 1.433(3) .
N1 C1 1.364(3) .
N1 C2 1.380(3) .
N1 C4 1.465(3) .
O3 C15 1.414(3) .
C4 C7 1.509(4) .
C4 C6 1.516(4) .
C4 H4A 1.0000 .
C2 C3 1.334(4) .
C2 H2A 0.9500 .
O2 C13 1.388(3) .
C3 H3A 0.9500 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C5 C9 1.511(4) .
C5 C8 1.525(4) .
C5 H5A 1.0000 .
C15 C16 1.498(4) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C13 C14 1.448(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C11 C12 1.500(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
