A mesoionic carbene stabilized nickel(II) hydroxide complex: a facile precursor for C-H activation chemistry.
Pavun, Anna; Niess, Raffael; Scheibel, Lucas A.; Seidl, Michael; Hohloch, Stephan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2749–2761; doi:10.1039/d3dt03746k

data_7714910
_publ_section_title
;
 A mesoionic carbene stabilized nickel(II) hydroxide complex: a facile
 precursor for C-H activation chemistry.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2749
_journal_page_last               2761
_journal_paper_doi               10.1039/d3dt03746k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H38 N10 Ni, C H2 Cl2'
_chemical_formula_sum            'C33 H40 Cl2 N10 Ni'
_chemical_formula_weight         706.36
_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             2022-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                77.721(7)
_cell_angle_beta                 85.348(7)
_cell_angle_gamma                79.973(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7265(16)
_cell_length_b                   13.252(2)
_cell_length_c                   16.223(3)
_cell_measurement_reflns_used    2439
_cell_measurement_temperature    103.00
_cell_measurement_theta_max      27.279
_cell_measurement_theta_min      2.241
_cell_volume                     1596.6(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      103.00
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 Quest, Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5579
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.241
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1083 before and 0.0859 after correction.
 The Ratio of minimum to maximum transmission is 0.76.

Final HKLF 4 output contains 41783 reflections, Rint = 0.0975
 (10413 with I > 3sig(I), Rint = 0.0508)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0022P)^2^+3.8208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5098
_reflns_number_total             5579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           sh_092n_0m_4
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_original_cell_volume        1596.7(5)
_cod_database_code               7714910
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.887
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6966(12)
 0.3034(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(H6BC)=Sof(H6BD)=Sof(H12C)=Sof(H12D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(H12A)=Sof(H12B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6AA,H6AB), C6(H6BC,H6BD), C11(H11A,H11B), C5(H5A,H5B), C9(H9A,H9B),
 C7(H7A,H7B), C12(H12A,H12B), C12(H12C,H12D), C100(H10E,H10F), C8(H8A,H8B),
 C10(H10A,H10B), C10A(H10C,H10D), C8A(H8AA,H8AB)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C15(H15), C22(H22), C17(H17)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              3293
_shelx_hkl_checksum              26767
_olex2_submission_special_instructions 'No special instructions were received'