#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:12:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179471 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/68/4336874.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_4336874
loop_
_publ_author_name
'Chun-Yi Lin'
'Jing-Dong Guo'
'James C. Fettinger'
'Shigeru Nagase'
'Fernande Grandjean'
'Gary J. Long'
'Nicholas F. Chilton'
'Philip P. Power'
_publ_section_title
;
 Dispersion Force Stabilized Two-Coordinate Transition Metal-Amido
 Complexes of the -N(SiMe3)Dipp (Dipp = C6H3-2,6-Pri2) Ligand: Structural,
 Spectroscopic, Magnetic, and Computational Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13584
_journal_page_last               13593
_journal_paper_doi               10.1021/ic402105m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H52 N2 Ni Si2'
_chemical_formula_sum            'C30 H52 N2 Ni Si2'
_chemical_formula_weight         555.62
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                102.0650(16)
_cell_angle_beta                 92.5472(17)
_cell_angle_gamma                114.3641(16)
_cell_formula_units_Z            1
_cell_length_a                   8.9104(13)
_cell_length_b                   9.1955(13)
_cell_length_c                   10.9978(16)
_cell_measurement_reflns_used    7252
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      2.51
_cell_volume                     794.0(2)
_computing_cell_refinement       'SAINT (7.68A) (Bruker, 2009)'
_computing_data_collection       'Apex2 (2010-11.3) (Bruker, 2010)'
_computing_data_reduction        'SAINT (7.68A) (Bruker, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.214
_diffrn_reflns_theta_min         1.914
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       Block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0418P)²+0.1336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3824
_reflns_number_total             4300
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic402105m_si_002_2.cif
_cod_data_source_block           CYL005
_cod_database_code               4336874
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 1.0000 1.0000 1.0000 0.01592(7) Uani 1 2 d S . P
Si1 Si 1.21627(4) 0.90175(4) 0.80828(3) 0.01709(8) Uani 1 1 d . . .
N1 N 1.04505(11) 0.93919(11) 0.84435(8) 0.01658(18) Uani 1 1 d . . .
C1 C 1.15615(16) 0.72800(16) 0.66490(12) 0.0266(3) Uani 1 1 d . . .
H1A H 1.0749 0.6263 0.6820 0.040 Uiso 1 1 calc R U .
H1B H 1.2553 0.7137 0.6424 0.040 Uiso 1 1 calc R U .
H1C H 1.1067 0.7528 0.5952 0.040 Uiso 1 1 calc R U .
C2 C 1.39392(15) 1.08479(15) 0.77860(12) 0.0240(2) Uani 1 1 d . . .
H2A H 1.3615 1.1083 0.7012 0.036 Uiso 1 1 calc R U .
H2B H 1.4910 1.0609 0.7697 0.036 Uiso 1 1 calc R U .
H2C H 1.4221 1.1808 0.8494 0.036 Uiso 1 1 calc R U .
C3 C 1.28641(16) 0.84737(16) 0.94837(12) 0.0276(3) Uani 1 1 d . . .
H3A H 1.3094 0.9363 1.0237 0.041 Uiso 1 1 calc R U .
H3B H 1.3878 0.8325 0.9357 0.041 Uiso 1 1 calc R U .
H3C H 1.1987 0.7448 0.9590 0.041 Uiso 1 1 calc R U .
C4 C 0.91153(13) 0.92299(13) 0.75703(10) 0.0161(2) Uani 1 1 d . . .
C5 C 0.76406(13) 0.77201(13) 0.72214(10) 0.0173(2) Uani 1 1 d . . .
C6 C 0.74682(14) 0.62393(13) 0.77195(11) 0.0199(2) Uani 1 1 d . . .
H6 H 0.8602 0.6454 0.8104 0.024 Uiso 1 1 calc R U .
C7 C 0.63502(17) 0.60485(16) 0.87580(12) 0.0287(3) Uani 1 1 d . . .
H7A H 0.6834 0.7052 0.9446 0.043 Uiso 1 1 calc R U .
H7B H 0.6268 0.5103 0.9076 0.043 Uiso 1 1 calc R U .
H7C H 0.5237 0.5869 0.8413 0.043 Uiso 1 1 calc R U .
C8 C 0.68108(16) 0.46335(14) 0.66723(12) 0.0260(2) Uani 1 1 d . . .
H8A H 0.5661 0.4339 0.6328 0.039 Uiso 1 1 calc R U .
H8B H 0.6844 0.3746 0.7018 0.039 Uiso 1 1 calc R U .
H8C H 0.7509 0.4792 0.6003 0.039 Uiso 1 1 calc R U .
C9 C 0.63044(14) 0.76179(14) 0.64316(11) 0.0211(2) Uani 1 1 d . . .
H9 H 0.5313 0.6618 0.6202 0.025 Uiso 1 1 calc R U .
C10 C 0.63998(15) 0.89513(15) 0.59758(12) 0.0234(2) Uani 1 1 d . . .
H10 H 0.5483 0.8859 0.5439 0.028 Uiso 1 1 calc R U .
C11 C 0.78475(15) 1.04208(15) 0.63124(11) 0.0220(2) Uani 1 1 d . . .
H11 H 0.7906 1.1329 0.6000 0.026 Uiso 1 1 calc R U .
C12 C 0.92185(14) 1.05910(13) 0.71001(10) 0.0182(2) Uani 1 1 d . . .
C13 C 1.07689(14) 1.22265(13) 0.74707(11) 0.0209(2) Uani 1 1 d . . .
H13 H 1.1677 1.2022 0.7858 0.025 Uiso 1 1 calc R U .
C14 C 1.13682(17) 1.29148(16) 0.63358(13) 0.0293(3) Uani 1 1 d . . .
H14A H 1.1481 1.2066 0.5692 0.044 Uiso 1 1 calc R U .
H14B H 1.2450 1.3877 0.6602 0.044 Uiso 1 1 calc R U .
H14C H 1.0557 1.3241 0.5988 0.044 Uiso 1 1 calc R U .
C15 C 1.04922(18) 1.34996(16) 0.84673(13) 0.0306(3) Uani 1 1 d . . .
H15A H 0.9562 1.3679 0.8134 0.046 Uiso 1 1 calc R U .
H15B H 1.1504 1.4542 0.8681 0.046 Uiso 1 1 calc R U .
H15C H 1.0235 1.3090 0.9222 0.046 Uiso 1 1 calc R U .
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'
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
N1 Ni1 N1 180.0 2_777
N1 Si1 C1 110.49(5) .
N1 Si1 C3 105.90(5) .
C1 Si1 C3 110.63(6) .
N1 Si1 C2 113.37(5) .
C1 Si1 C2 107.56(6) .
C3 Si1 C2 108.89(6) .
C4 N1 Si1 126.82(7) .
C4 N1 Ni1 107.13(7) .
Si1 N1 Ni1 126.02(5) .
Si1 C1 H1A 109.5 .
Si1 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
Si1 C1 H1C 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
Si1 C2 H2A 109.5 .
Si1 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
Si1 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
Si1 C3 H3A 109.5 .
Si1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
Si1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C12 C4 C5 119.82(10) .
C12 C4 N1 120.45(9) .
C5 C4 N1 119.65(9) .
C9 C5 C4 118.91(10) .
C9 C5 C6 119.54(10) .
C4 C5 C6 121.51(10) .
C5 C6 C8 112.43(10) .
C5 C6 C7 110.56(10) .
C8 C6 C7 110.61(10) .
C5 C6 H6 107.7 .
C8 C6 H6 107.7 .
C7 C6 H6 107.7 .
C6 C7 H7A 109.5 .
C6 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C6 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
C6 C8 H8A 109.5 .
C6 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C6 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C10 C9 C5 121.34(11) .
C10 C9 H9 119.3 .
C5 C9 H9 119.3 .
C9 C10 C11 119.54(11) .
C9 C10 H10 120.2 .
C11 C10 H10 120.2 .
C10 C11 C12 121.47(11) .
C10 C11 H11 119.3 .
C12 C11 H11 119.3 .
C11 C12 C4 118.89(10) .
C11 C12 C13 120.09(10) .
C4 C12 C13 120.99(10) .
C12 C13 C14 112.52(10) .
C12 C13 C15 111.21(10) .
C14 C13 C15 110.66(10) .
C12 C13 H13 107.4 .
C14 C13 H13 107.4 .
C15 C13 H13 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 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.8028(9) 2_777
Ni1 N1 1.8029(10) .
Si1 N1 1.7417(10) .
Si1 C1 1.8686(13) .
Si1 C3 1.8732(12) .
Si1 C2 1.8769(12) .
N1 C4 1.4326(13) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C12 1.4220(15) .
C4 C5 1.4243(15) .
C5 C9 1.4009(15) .
C5 C6 1.5247(15) .
C6 C8 1.5380(16) .
C6 C7 1.5389(17) .
C6 H6 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C10 1.3916(17) .
C9 H9 0.9500 .
C10 C11 1.3919(17) .
C10 H10 0.9500 .
C11 C12 1.3996(16) .
C11 H11 0.9500 .
C12 C13 1.5218(15) .
C13 C14 1.5343(17) .
C13 C15 1.5357(17) .
C13 H13 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
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
C1 Si1 N1 C4 -34.31(11)
C3 Si1 N1 C4 -154.15(9)
C2 Si1 N1 C4 86.52(10)
C1 Si1 N1 Ni1 143.68(7)
C3 Si1 N1 Ni1 23.83(8)
C2 Si1 N1 Ni1 -95.49(7)
Si1 N1 C4 C12 -90.15(12)
Ni1 N1 C4 C12 91.55(10)
Si1 N1 C4 C5 93.04(12)
Ni1 N1 C4 C5 -85.25(10)
C12 C4 C5 C9 -0.98(16)
N1 C4 C5 C9 175.85(10)
C12 C4 C5 C6 -179.08(10)
N1 C4 C5 C6 -2.26(15)
C9 C5 C6 C8 49.73(14)
C4 C5 C6 C8 -132.17(11)
C9 C5 C6 C7 -74.42(13)
C4 C5 C6 C7 103.67(12)
C4 C5 C9 C10 0.65(17)
C6 C5 C9 C10 178.79(11)
C5 C9 C10 C11 -0.22(18)
C9 C10 C11 C12 0.13(18)
C10 C11 C12 C4 -0.47(17)
C10 C11 C12 C13 -178.75(11)
C5 C4 C12 C11 0.89(16)
N1 C4 C12 C11 -175.91(10)
C5 C4 C12 C13 179.16(10)
N1 C4 C12 C13 2.36(16)
C11 C12 C13 C14 -49.17(15)
C4 C12 C13 C14 132.58(11)
C11 C12 C13 C15 75.63(14)
C4 C12 C13 C15 -102.62(12)
