#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:16:20 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178556 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/64/4066442.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_4066442
loop_
_publ_author_name
'Yang, Jian'
'Del Rosal, Iker'
'Fasulo, Meg'
'Sangtrirutnugul, Preeyanuch'
'Maron, Laurent'
'Tilley, T. Don'
_publ_section_title
;
 Nickel Complexes with Bis(8-quinolyl)silyl Ligands. An Unusual
 Ni3Si2Cluster Containing Six-Coordinate Silicon†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5544
_journal_paper_doi               10.1021/om1004622
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C25 H47 Cl4 N3 Ni'
_chemical_formula_sum            'C25 H47 Cl4 N3 Ni'
_chemical_formula_weight         590.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.4381(11)
_cell_length_b                   14.4903(6)
_cell_length_c                   7.8339(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.324
_cell_measurement_theta_min      1.704
_cell_volume                     3114.7(2)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω 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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            44513
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.9290
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0342
_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)+(0.0487P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                2403
_reflns_number_total             2972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1004622_si_002.cif
_cod_data_source_block           jian3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4066442
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Ni1 Ni 0.683087(15) -0.2500 0.01458(6) 0.02940(15) Uani 1 2 d S
Cl1 Cl 0.42202(3) -0.2500 0.66028(10) 0.02714(19) Uani 1 2 d S
Cl3 Cl 0.66706(2) -0.12067(4) -0.13293(8) 0.03771(18) Uani 1 1 d .
Cl4 Cl 0.75417(3) -0.2500 0.15284(14) 0.0476(3) Uani 1 2 d S
N1 N 0.63194(10) -0.2500 0.2016(4) 0.0281(6) Uani 1 2 d S
N2 N 0.37209(7) -0.05469(12) 0.6273(2) 0.0249(4) Uani 1 1 d .
C1 C 0.58253(12) -0.2500 0.1702(4) 0.0274(7) Uani 1 2 d S
C2 C 0.56512(13) -0.2500 0.0006(4) 0.0346(8) Uani 1 2 d S
H2A H 0.5869 -0.2500 -0.0903 0.042 Uiso 1 2 calc SR
C3 C 0.51618(13) -0.2500 -0.0292(5) 0.0428(9) Uani 1 2 d S
H3A H 0.5050 -0.2500 -0.1414 0.051 Uiso 1 2 calc SR
C4 C 0.48241(13) -0.2500 0.1032(6) 0.0445(10) Uani 1 2 d S
H4A H 0.4492 -0.2500 0.0789 0.053 Uiso 1 2 calc SR
C5 C 0.49773(13) -0.2500 0.2671(5) 0.0411(9) Uani 1 2 d S
H5A H 0.4750 -0.2500 0.3550 0.049 Uiso 1 2 calc SR
C6 C 0.54802(12) -0.2500 0.3063(4) 0.0296(7) Uani 1 2 d S
C7 C 0.56571(15) -0.2500 0.4748(5) 0.0409(9) Uani 1 2 d S
H7A H 0.5440 -0.2500 0.5661 0.049 Uiso 1 2 calc SR
C8 C 0.61498(15) -0.2500 0.5044(5) 0.0400(9) Uani 1 2 d S
H8A H 0.6273 -0.2500 0.6151 0.048 Uiso 1 2 calc SR
C9 C 0.64628(13) -0.2500 0.3630(4) 0.0315(8) Uani 1 2 d S
H9A H 0.6796 -0.2500 0.3841 0.038 Uiso 1 2 calc SR
C10 C 0.38301(8) -0.02794(15) 0.4432(3) 0.0289(5) Uani 1 1 d .
H10A H 0.3675 0.0317 0.4202 0.035 Uiso 1 1 calc R
C11 C 0.36277(10) -0.09781(16) 0.3187(3) 0.0405(6) Uani 1 1 d .
H11A H 0.3283 -0.1037 0.3357 0.061 Uiso 1 1 calc R
H11B H 0.3782 -0.1565 0.3373 0.061 Uiso 1 1 calc R
H11C H 0.3690 -0.0776 0.2041 0.061 Uiso 1 1 calc R
C12 C 0.43751(9) -0.01727(17) 0.4171(4) 0.0408(6) Uani 1 1 d .
H12A H 0.4439 0.0000 0.3009 0.061 Uiso 1 1 calc R
H12B H 0.4534 -0.0747 0.4416 0.061 Uiso 1 1 calc R
H12C H 0.4497 0.0297 0.4922 0.061 Uiso 1 1 calc R
C13 C 0.31853(8) -0.07642(15) 0.6594(3) 0.0309(5) Uani 1 1 d .
H13A H 0.3089 -0.1246 0.5783 0.037 Uiso 1 1 calc R
C14 C 0.31203(9) -0.11518(17) 0.8368(4) 0.0421(7) Uani 1 1 d .
H14A H 0.2782 -0.1285 0.8560 0.063 Uiso 1 1 calc R
H14B H 0.3230 -0.0708 0.9192 0.063 Uiso 1 1 calc R
H14C H 0.3307 -0.1709 0.8479 0.063 Uiso 1 1 calc R
C15 C 0.28658(9) 0.00680(18) 0.6256(4) 0.0475(7) Uani 1 1 d .
H15A H 0.2918 0.0281 0.5111 0.071 Uiso 1 1 calc R
H15B H 0.2947 0.0551 0.7046 0.071 Uiso 1 1 calc R
H15C H 0.2530 -0.0100 0.6398 0.071 Uiso 1 1 calc R
C16 C 0.39209(8) 0.01562(14) 0.7521(3) 0.0299(5) Uani 1 1 d .
H16A H 0.3665 0.0330 0.8312 0.036 Uiso 1 1 calc R
H16B H 0.4017 0.0705 0.6898 0.036 Uiso 1 1 calc R
C17 C 0.43547(9) -0.01982(17) 0.8523(3) 0.0407(6) Uani 1 1 d .
H17A H 0.4466 0.0273 0.9292 0.061 Uiso 1 1 calc R
H17B H 0.4613 -0.0358 0.7750 0.061 Uiso 1 1 calc R
H17C H 0.4261 -0.0734 0.9163 0.061 Uiso 1 1 calc R
H1 H 0.3868(8) -0.1037(14) 0.639(3) 0.018(6) Uiso 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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
N1 Ni1 Cl4 104.72(8) .
N1 Ni1 Cl3 103.67(4) .
Cl4 Ni1 Cl3 114.91(2) .
N1 Ni1 Cl3 103.67(4) 7
Cl4 Ni1 Cl3 114.90(2) 7
Cl3 Ni1 Cl3 113.17(4) 7
C9 N1 C1 117.6(3) .
C9 N1 Ni1 118.9(2) .
C1 N1 Ni1 123.5(2) .
C16 N2 C10 111.64(16) .
C16 N2 C13 112.44(17) .
C10 N2 C13 113.49(17) .
C16 N2 H1 109.3(15) .
C10 N2 H1 103.3(15) .
C13 N2 H1 106.1(15) .
N1 C1 C2 120.1(3) .
N1 C1 C6 121.3(3) .
C2 C1 C6 118.6(3) .
C3 C2 C1 119.6(3) .
C3 C2 H2A 120.2 .
C1 C2 H2A 120.2 .
C2 C3 C4 121.9(4) .
C2 C3 H3A 119.1 .
C4 C3 H3A 119.1 .
C5 C4 C3 120.1(4) .
C5 C4 H4A 119.9 .
C3 C4 H4A 119.9 .
C4 C5 C6 120.7(3) .
C4 C5 H5A 119.7 .
C6 C5 H5A 119.7 .
C7 C6 C5 122.7(3) .
C7 C6 C1 118.2(3) .
C5 C6 C1 119.1(3) .
C8 C7 C6 119.9(3) .
C8 C7 H7A 120.0 .
C6 C7 H7A 120.0 .
C7 C8 C9 118.1(3) .
C7 C8 H8A 121.0 .
C9 C8 H8A 121.0 .
N1 C9 C8 124.9(3) .
N1 C9 H9A 117.5 .
C8 C9 H9A 117.5 .
C11 C10 C12 110.1(2) .
C11 C10 N2 111.60(18) .
C12 C10 N2 110.33(19) .
C11 C10 H10A 108.2 .
C12 C10 H10A 108.2 .
N2 C10 H10A 108.2 .
C10 C11 H11A 109.5 .
C10 C11 H11B 109.5 .
H11A C11 H11B 109.5 .
C10 C11 H11C 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C10 C12 H12A 109.5 .
C10 C12 H12B 109.5 .
H12A C12 H12B 109.5 .
C10 C12 H12C 109.5 .
H12A C12 H12C 109.5 .
H12B C12 H12C 109.5 .
C14 C13 C15 112.9(2) .
C14 C13 N2 110.05(19) .
C15 C13 N2 111.41(18) .
C14 C13 H13A 107.4 .
C15 C13 H13A 107.4 .
N2 C13 H13A 107.4 .
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 .
C13 C15 H15A 109.5 .
C13 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C13 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
N2 C16 C17 113.02(18) .
N2 C16 H16A 109.0 .
C17 C16 H16A 109.0 .
N2 C16 H16B 109.0 .
C17 C16 H16B 109.0 .
H16A C16 H16B 107.8 .
C16 C17 H17A 109.5 .
C16 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C16 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.029(3) .
Ni1 Cl4 2.2309(10) .
Ni1 Cl3 2.2452(6) .
Ni1 Cl3 2.2452(6) 7
N1 C9 1.324(4) .
N1 C1 1.378(4) .
N2 C16 1.515(3) .
N2 C10 1.523(3) .
N2 C13 1.524(3) .
N2 H1 0.82(2) .
C1 C2 1.412(5) .
C1 C6 1.426(5) .
C2 C3 1.363(5) .
C2 H2A 0.9300 .
C3 C4 1.391(5) .
C3 H3A 0.9300 .
C4 C5 1.350(6) .
C4 H4A 0.9300 .
C5 C6 1.414(5) .
C5 H5A 0.9300 .
C6 C7 1.407(5) .
C7 C8 1.372(5) .
C7 H7A 0.9300 .
C8 C9 1.402(5) .
C8 H8A 0.9300 .
C9 H9A 0.9300 .
C10 C11 1.511(3) .
C10 C12 1.517(3) .
C10 H10A 0.9800 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.510(4) .
C13 C15 1.514(3) .
C13 H13A 0.9800 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C17 1.516(3) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Cl4 Ni1 N1 C9 0.0 .
Cl3 Ni1 N1 C9 -120.79(3) .
Cl3 Ni1 N1 C9 120.79(3) 7
Cl4 Ni1 N1 C1 180.0 .
Cl3 Ni1 N1 C1 59.21(3) .
Cl3 Ni1 N1 C1 -59.21(3) 7
C9 N1 C1 C2 180.0 .
Ni1 N1 C1 C2 0.0 .
C9 N1 C1 C6 0.0 .
Ni1 N1 C1 C6 180.0 .
N1 C1 C2 C3 180.0 .
C6 C1 C2 C3 0.0 .
C1 C2 C3 C4 0.0 .
C2 C3 C4 C5 0.0 .
C3 C4 C5 C6 0.0 .
C4 C5 C6 C7 180.0 .
C4 C5 C6 C1 0.0 .
N1 C1 C6 C7 0.0 .
C2 C1 C6 C7 180.0 .
N1 C1 C6 C5 180.0 .
C2 C1 C6 C5 0.0 .
C5 C6 C7 C8 180.0 .
C1 C6 C7 C8 0.0 .
C6 C7 C8 C9 0.0 .
C1 N1 C9 C8 0.0 .
Ni1 N1 C9 C8 180.0 .
C7 C8 C9 N1 0.0 .
C16 N2 C10 C11 -179.63(19) .
C13 N2 C10 C11 -51.3(2) .
C16 N2 C10 C12 57.6(2) .
C13 N2 C10 C12 -174.04(18) .
C16 N2 C13 C14 -60.2(2) .
C10 N2 C13 C14 171.92(18) .
C16 N2 C13 C15 65.8(3) .
C10 N2 C13 C15 -62.1(3) .
C10 N2 C16 C17 -109.0(2) .
C13 N2 C16 C17 122.1(2) .
