Synthesis and reactivity of a -1,2-dinitrogen dinickel(II) complex with C-H activated silaamidinate pincer ligand
Hu , Chaopeng; Ding, Yazhou; Bai, Yunping; Guo, Lulu; Cui, Chunming; Chemical Communications  (2022) –; doi:10.1039/D2CC05472H

data_7131020
_publ_section_title
;
 Synthesis and reactivity of a &#xF06D;-1,2-dinitrogen dinickel(II)
 complex with C-H activated silaamidinate pincer ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05472H
_journal_year                    2022
_chemical_formula_moiety         'C78 H112 N10 Ni2 Si2'
_chemical_formula_sum            'C78 H112 N10 Ni2 Si2'
_chemical_formula_weight         1363.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-06 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.515(5)
_cell_angle_beta                 111.529(5)
_cell_angle_gamma                96.493(4)
_cell_formula_units_Z            2
_cell_length_a                   15.2773(9)
_cell_length_b                   16.5998(8)
_cell_length_c                   18.2805(10)
_cell_measurement_temperature    113.15
_cell_volume                     4090.5(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.1412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43838
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.942
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86751
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         16704
_refine_ls_number_restraints     2427
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9592
_reflns_number_total             16704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05472h2.cif
_cod_data_source_block           hcpnin2
_cod_depositor_comments
;

2025-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C9.11 H12.67 N1.11 Ni0.22 O0.11 Si0.22'
_cod_original_formula_weight         158.83
_cod_original_formula_moiety         '0.11(C78 H112 N10 Ni2 Si2)'
_cod_original_formula_units_Z            18
_cod_database_code               7131020
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C0aa \\sim C00T \\sim C00Y \\sim C1 \\sim C01C \\sim C01G \\sim C01J \\sim C01L
\\sim C01M \\sim C01O \\sim C01R \\sim C01S \\sim C01T \\sim C01U \\sim C01W
\\sim C01X \\sim C01Z \\sim C2 \\sim C02A \\sim C02B \\sim C02E \\sim C02F
\\sim C02G \\sim C02H \\sim C02K \\sim C02L \\sim C02N \\sim C3 \\sim C4 \\sim
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C010 \\sim C10 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C016 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim
C020 \\sim C20 \\sim C21 \\sim C021 \\sim C22 \\sim C022 \\sim C23 \\sim C023
\\sim C024 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C027 \\sim C028 \\sim
C28 \\sim C029 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42
\\sim C43 \\sim C44: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C19(H19), C20(H20), C27(H27), C28(H28)
4.b Aromatic/amide H refined with riding coordinates:
 C01C(H01C), C01G(H01G), C01J(H01J), C01R(H01R), C01S(H01S), C02F(H02j),
 C010(H010), C14(H14), C15(H15), C016(H016), C16(H16), C021(H021), C23(H23),
 C24(H24), C25(H25), C027(H027), C34(H34), C35(H35), C36(H36), C41(H41),
 C42(H42), C43(H43)
4.c Idealised Me refined as rotating group:
 C01L(H01a,H01b,H01d), C01M(H01e,H01f,H01h), C01O(H01i,H01k,H01l), C01T(H01m,
 H01n,H01o), C01U(H01p,H01q,H01t), C01W(H01u,H01v,H01w), C01X(H01x,H01y,H),
 C01Z(H01z,Ha,Hb), C02A(H02a,H02b,H02c), C02B(H02d,H02e,H02f), C02E(H02g,H02h,
 H02i), C02G(H02k,H02l,H02m), C02H(H02n,H02o,H02p), C02K(H02q,H02r,H02s),
 C02L(H02t,H02u,H02v), C02N(H02w,H02x,H02y), C12(H12a,H12b,H12c), C13(H13a,H13b,
 H13c), C020(H02z,Hc,Hd), C022(H02,He,Hf), C023(H0aa,Hg,Hh), C024(H1aa,Hi,Hj),
 C028(H2aa,Hk,Hl), C029(H3aa,Hm,Hn), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c),
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c)
;
_shelx_res_checksum              39603
_shelx_hkl_checksum              90618
_shelx_fab_checksum              6111
_olex2_submission_special_instructions 'No special instructions were received'