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_7131018
_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         'C48 H65 N5 Ni Si'
_chemical_formula_sum            'C48 H65 N5 Ni Si'
_chemical_formula_weight         798.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-09-06 deposited with the CCDC.	2022-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.380(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.045(2)
_cell_length_b                   12.0991(16)
_cell_length_c                   15.7064(15)
_cell_measurement_reflns_used    6461
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      29.5640
_cell_measurement_theta_min      2.1160
_cell_volume                     4494.6(8)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  35.00   1.00    2.00    --  -25.00  45.00  90.00  150
  3  \w   -115.00   5.00   1.00    2.00    --  -25.00  45.00 180.00  120
;
_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      -0.0027935000
_diffrn_orient_matrix_UB_12      0.0572135000
_diffrn_orient_matrix_UB_13      0.0082100000
_diffrn_orient_matrix_UB_21      -0.0295199000
_diffrn_orient_matrix_UB_22      -0.0066585000
_diffrn_orient_matrix_UB_23      -0.0021590000
_diffrn_orient_matrix_UB_31      0.0045944000
_diffrn_orient_matrix_UB_32      -0.0108993000
_diffrn_orient_matrix_UB_33      0.0450973000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1771
_diffrn_reflns_av_unetI/netI     0.1505
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32119
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.149
_diffrn_reflns_theta_max         24.149
_diffrn_reflns_theta_min         1.722
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63435
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     4087
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.1081
_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^)+(0.0860P)^2^+19.5313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2358
_refine_ls_wR_factor_ref         0.2783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3965
_reflns_number_total             7168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05472h2.cif
_cod_data_source_block           r20210625c
_cod_original_cell_volume        4494.6(9)
_cod_database_code               7131018
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.907
_reflns_odcompleteness_completeness 99.88
_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
2. Rigid bond restraints
 N4, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C43 \\sim C35 \\sim C2 \\sim C16 \\sim C12 \\sim C14 \\sim C17 \\sim C11 \\sim
C13 \\sim C48 \\sim C20 \\sim C46 \\sim C39 \\sim C44 \\sim C15 \\sim C45 \\sim
C47 \\sim C23 \\sim C36 \\sim C37 \\sim C38 \\sim C22 \\sim C42 \\sim C28 \\sim
C25 \\sim C1 \\sim C19 \\sim C24 \\sim C21 \\sim C26 \\sim C29 \\sim C18 \\sim
C41 \\sim C40 \\sim C27 \\sim C30 \\sim C32 \\sim C3 \\sim C8 \\sim C31 \\sim
C4 \\sim C33 \\sim C34 \\sim C9 \\sim C10 \\sim C7 \\sim C5 \\sim C6: within
7.2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 7.2A
Uanis(Ni1) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C17(H17), C29(H29), C32(H32)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C48(H48), C46(H46), C44(H44), C15(H15), C45(H45),
 C47(H47), C25(H25), C26(H26), C27(H27), C7(H7), C5(H5), C6(H6)
4.c Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C22(H22a,H22b,
 H22c), C42(H42a,H42b,H42c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C18(H18a,
 H18b,H18c), C41(H41a,H41b,H41c), C40(H40a,H40b,H40c), C30(H30a,H30b,H30c),
 C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C9(H9a,H9b,H9c),
  C10(H10a,H10b,H10c)
;
_shelx_res_checksum              10693
_shelx_hkl_checksum              73541
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.793