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_7131019
_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         'C40 H57 Li N4 Ni O Si'
_chemical_formula_sum            'C40 H57 Li N4 Ni O Si'
_chemical_formula_weight         703.63
_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     dual
_audit_creation_date             2021-06-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-06 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                73.179(3)
_cell_angle_beta                 73.148(3)
_cell_angle_gamma                67.295(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4166(3)
_cell_length_b                   12.1080(5)
_cell_length_c                   16.0882(6)
_cell_measurement_reflns_used    13888
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      32.4780
_cell_measurement_theta_min      1.9000
_cell_volume                     1923.38(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0571259000
_diffrn_orient_matrix_UB_12      -0.0347183000
_diffrn_orient_matrix_UB_13      -0.0073512000
_diffrn_orient_matrix_UB_21      0.0179718000
_diffrn_orient_matrix_UB_22      -0.0189559000
_diffrn_orient_matrix_UB_23      0.0243133000
_diffrn_orient_matrix_UB_31      -0.0268816000
_diffrn_orient_matrix_UB_32      0.0254322000
_diffrn_orient_matrix_UB_33      0.0201350000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.910
_diffrn_reflns_theta_min         1.861
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         12891
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0701
_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/[\s^2^(Fo^2^)+(0.0951P)^2^+1.4793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8285
_reflns_number_total             12891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05472h2.cif
_cod_data_source_block           hcp210607
_cod_database_code               7131019
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C40A-C37A = C37A-C39A
 1.54 with sigma of 0.02
 C40-C37 = C37-C39
 1.54 with sigma of 0.02
 C39-C37 = C37-C38
 1.54 with sigma of 0.02
 C38-C37 = C37-C40
 1.54 with sigma of 0.02
 C39A-C37A = C37A-C38
 1.54 with sigma of 0.02
 C38-C37A = C37A-C40A
 1.54 with sigma of 0.02
 C40-C39
 2.515 with sigma of 0.04
 C38-C40A
 2.515 with sigma of 0.04
 C38-C40
 2.515 with sigma of 0.04
 C39-C38
 2.515 with sigma of 0.04
 C39A-C38
 2.515 with sigma of 0.04
 C40A-C39A
 2.515 with sigma of 0.04
 N4-C37A \\sim N4-C37
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N4, C37, C38, C40, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C37A, C38, C39A, C40A, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C36, C32, C33, C35, C31, C34, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C33A, C31A, C36A, C34A, C32A, C35A, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C37A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=
 Sof(H40F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(C37)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(2)
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C20(H20), C23(H23)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5A(H5A), C6(H6), C16(H16), C17(H17), C18(H18), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A),
 C36A(H36A)
5.c Fitted hexagon refined as free rotating group:
 C31(C32,C33,C34,C35,C36), C31A(C32A,C33A,C34A,C35A,C36A)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C38(H38A,H38B,H38C), C38(H38D,H38E,H38F), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C40A(H40D,H40E,H40F), C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              94399
_shelx_hkl_checksum              59339
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.622
_oxdiff_exptl_absorpt_empirical_full_min 0.353