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_7131017
_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         'C47 H75 Br2 Li N4 Ni O2 Si'
_chemical_formula_sum            'C47 H75 Br2 Li N4 Ni O2 Si'
_chemical_formula_weight         981.67
_chemical_name_systematic        NiBr
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-19
_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                 104.114(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4789(11)
_cell_length_b                   16.6281(8)
_cell_length_c                   21.2921(10)
_cell_measurement_reflns_used    12599
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      30.7120
_cell_measurement_theta_min      1.7560
_cell_volume                     6001.5(6)
_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)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.572
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38671
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         12273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0678P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7320
_reflns_number_total             12273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05472h2.cif
_cod_data_source_block           r20210819a_sq
_cod_database_code               7131017
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.726
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00Y(H00Y), C010(H010), C011(H011)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00Q(H00Q), C00R(H00R), C014(H014), C016(H016), C019(H019)
2.d Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00C), C00W(H00D,H00E,H00F), C00Z(H00N,H00O,H00P), C012(H01A,
 H01B,H01C), C013(H01D,H01E,H01F), C015(H01G,H01H,H01I), C017(H01J,H01K,H01L),
 C018(H01M,H01N,H01O), C01A(H01P,H01Q,H01R), C01B(H01S,H01T,H01U), C01C(H01V,
 H01W,H01X), C01F(H01Y,H,HA), C01M(H01Z,HB,HC), C01O(H01,HD,HE), C1(H1A,H1B,
 H1C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              40437
_shelx_hkl_checksum              26957
_shelx_fab_checksum              48430
_olex2_submission_special_instructions 'No special instructions were received'