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_7714914
_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         'C39 H46 N8 Ni O2 S, 1[C6H6]'
_chemical_formula_sum            'C45 H52 N8 Ni O2 S'
_chemical_formula_weight         827.71
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-21
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.097(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3158(15)
_cell_length_b                   21.3714(16)
_cell_length_c                   12.1193(11)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      21.953
_cell_measurement_theta_min      2.211
_cell_volume                     4202.0(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest, PhotonIII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1362
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            95811
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.906
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.8834.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0815P)^2^+1.8251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5626
_reflns_number_total             7819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           sh_130m
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_database_code               7714914
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.807
_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. Others
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C7(H7A,H7B), C9(H9A,H9B), C12(H12A,H12B), C6(H6A,
 H6B), C10(H10A,H10B), C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C15(H15), C17(H17), C20(H20), C41(H41), C45(H45), C42(H42), C44(H44)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C46(H46A,H46B,
 H46C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C27A(H27D,H27E,H27F), C28A(H28D,H28E,H28F), C26A(H26D,H26E,H26F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 870\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C6H6] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9882
_shelx_hkl_checksum              42000
_shelx_fab_checksum              94960
_olex2_submission_special_instructions 'No special instructions were received'