#------------------------------------------------------------------------------
#$Date: 2025-08-22 00:26:11 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/79/7107979.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_7107979
loop_
_publ_author_name
'Michael Lipschutz'
'T.Don Tilley'
_publ_section_title
;
 Synthesis and reactivity of a conveniently prepared two-coordinate
 bis(amido) nickel(II) complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              7146
_journal_paper_doi               10.1039/c2cc32974c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C30 H52 N2 Ni Si2'
_chemical_formula_weight         555.62
_chemical_name_common            Ni(N(SiMe3)(DIPP))2
_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           SHELXL-97
_cell_angle_alpha                102.092(2)
_cell_angle_beta                 92.571(2)
_cell_angle_gamma                114.391(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9248(4)
_cell_length_b                   9.1680(4)
_cell_length_c                   10.9493(5)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.52
_cell_volume                     789.11(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.9196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0241
_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)+(0.0321P)²+0.3414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                2713
_reflns_number_total             2891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32974c.txt
_cod_data_source_block           shelxl_a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107979
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
C1 C 0.58800(17) 0.07697(17) 0.24294(12) 0.0154(3) Uani 1 1 d .
C2 C 0.73548(17) 0.22771(17) 0.27750(13) 0.0164(3) Uani 1 1 d .
C3 C 0.86820(18) 0.23724(18) 0.35601(13) 0.0203(3) Uani 1 1 d .
H3 H 0.9673 0.3375 0.3790 0.024 Uiso 1 1 calc R
C4 C 0.85905(19) 0.10402(19) 0.40128(14) 0.0221(3) Uani 1 1 d .
H4 H 0.9509 0.1129 0.4547 0.026 Uiso 1 1 calc R
C5 C 0.71428(19) -0.04265(19) 0.36780(14) 0.0215(3) Uani 1 1 d .
H5 H 0.7081 -0.1339 0.3990 0.026 Uiso 1 1 calc R
C6 C 0.57811(18) -0.05901(17) 0.28965(13) 0.0175(3) Uani 1 1 d .
C7 C 0.42270(19) -0.22276(17) 0.25268(14) 0.0199(3) Uani 1 1 d .
H7 H 0.3324 -0.2020 0.2135 0.024 Uiso 1 1 calc R
C8 C 0.4494(2) -0.35104(19) 0.15332(15) 0.0290(4) Uani 1 1 d .
H8A H 0.5416 -0.3698 0.1872 0.044 Uiso 1 1 calc R
H8B H 0.4759 -0.3103 0.0774 0.044 Uiso 1 1 calc R
H8C H 0.3479 -0.4552 0.1317 0.044 Uiso 1 1 calc R
C9 C 0.3627(2) -0.29035(19) 0.36692(15) 0.0279(4) Uani 1 1 d .
H9A H 0.4437 -0.3226 0.4025 0.042 Uiso 1 1 calc R
H9B H 0.2548 -0.3871 0.3404 0.042 Uiso 1 1 calc R
H9C H 0.3514 -0.2047 0.4310 0.042 Uiso 1 1 calc R
C10 C 0.75278(18) 0.37591(17) 0.22786(13) 0.0190(3) Uani 1 1 d .
H10 H 0.6396 0.3544 0.1892 0.023 Uiso 1 1 calc R
C11 C 0.8185(2) 0.53667(18) 0.33309(15) 0.0253(3) Uani 1 1 d .
H11A H 0.7480 0.5210 0.3998 0.038 Uiso 1 1 calc R
H11B H 0.8164 0.6261 0.2983 0.038 Uiso 1 1 calc R
H11C H 0.9329 0.5655 0.3683 0.038 Uiso 1 1 calc R
C12 C 0.8644(2) 0.3956(2) 0.12392(15) 0.0278(4) Uani 1 1 d .
H12A H 0.9755 0.4134 0.1586 0.042 Uiso 1 1 calc R
H12B H 0.8728 0.4907 0.0923 0.042 Uiso 1 1 calc R
H12C H 0.8161 0.2952 0.0545 0.042 Uiso 1 1 calc R
C13 C 0.10746(19) -0.08443(18) 0.22154(15) 0.0226(3) Uani 1 1 d .
H13A H 0.0786 -0.1807 0.1502 0.034 Uiso 1 1 calc R
H13B H 0.0109 -0.0602 0.2312 0.034 Uiso 1 1 calc R
H13C H 0.1403 -0.1083 0.2989 0.034 Uiso 1 1 calc R
C14 C 0.2139(2) 0.1519(2) 0.05109(15) 0.0260(3) Uani 1 1 d .
H14A H 0.3015 0.2546 0.0400 0.039 Uiso 1 1 calc R
H14B H 0.1127 0.1670 0.0638 0.039 Uiso 1 1 calc R
H14C H 0.1906 0.0623 -0.0244 0.039 Uiso 1 1 calc R
C15 C 0.3440(2) 0.27244(19) 0.33496(15) 0.0258(3) Uani 1 1 d .
H15A H 0.3927 0.2474 0.4053 0.039 Uiso 1 1 calc R
H15B H 0.2451 0.2873 0.3571 0.039 Uiso 1 1 calc R
H15C H 0.4257 0.3742 0.3179 0.039 Uiso 1 1 calc R
N1 N 0.45461(14) 0.06117(14) 0.15574(10) 0.0156(2) Uani 1 1 d .
Si1 Si 0.28409(5) 0.09839(5) 0.19158(3) 0.01601(11) Uani 1 1 d .
Ni1 Ni 0.5000 0.0000 0.0000 0.01491(9) Uani 1 2 d S
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
C6 C1 C2 119.66(13) .
C6 C1 N1 120.60(12) .
C2 C1 N1 119.65(12) .
C3 C2 C1 118.83(13) .
C3 C2 C10 119.66(13) .
C1 C2 C10 121.49(13) .
C4 C3 C2 121.58(13) .
C4 C3 H3 119.2 .
C2 C3 H3 119.2 .
C3 C4 C5 119.33(14) .
C3 C4 H4 120.3 .
C5 C4 H4 120.3 .
C4 C5 C6 121.49(14) .
C4 C5 H5 119.3 .
C6 C5 H5 119.3 .
C5 C6 C1 119.10(13) .
C5 C6 C7 120.08(13) .
C1 C6 C7 120.81(13) .
C6 C7 C8 111.25(12) .
C6 C7 C9 112.40(12) .
C8 C7 C9 110.77(12) .
C6 C7 H7 107.4 .
C8 C7 H7 107.4 .
C9 C7 H7 107.4 .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C7 C9 H9A 109.5 .
C7 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C7 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C2 C10 C11 112.43(12) .
C2 C10 C12 110.66(12) .
C11 C10 C12 110.48(12) .
C2 C10 H10 107.7 .
C11 C10 H10 107.7 .
C12 C10 H10 107.7 .
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 .
Si1 C13 H13A 109.5 .
Si1 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
Si1 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
Si1 C14 H14A 109.5 .
Si1 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
Si1 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
Si1 C15 H15A 109.5 .
Si1 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
Si1 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C1 N1 Si1 127.16(9) .
C1 N1 Ni1 106.66(9) .
Si1 N1 Ni1 126.16(7) .
N1 Si1 C15 110.44(6) .
N1 Si1 C14 105.94(7) .
C15 Si1 C14 110.70(8) .
N1 Si1 C13 113.40(6) .
C15 Si1 C13 107.53(7) .
C14 Si1 C13 108.83(7) .
N1 Ni1 N1 180.00(8) 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.416(2) .
C1 C2 1.421(2) .
C1 N1 1.4309(18) .
C2 C3 1.393(2) .
C2 C10 1.519(2) .
C3 C4 1.385(2) .
C3 H3 0.9500 .
C4 C5 1.388(2) .
C4 H4 0.9500 .
C5 C6 1.391(2) .
C5 H5 0.9500 .
C6 C7 1.522(2) .
C7 C8 1.531(2) .
C7 C9 1.532(2) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.535(2) .
C10 C12 1.536(2) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 Si1 1.8699(15) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 Si1 1.8666(15) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 Si1 1.8620(15) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
N1 Si1 1.7358(12) .
N1 Ni1 1.7987(11) .
Ni1 N1 1.7987(11) 2_655
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139140502
