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_7714919
_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         'C42 H41 F6 N7 Ni, 2[C7H8]'
_chemical_formula_sum            'C56 H57 F6 N7 Ni'
_chemical_formula_weight         1000.79
_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             2023-05-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                67.512(2)
_cell_angle_beta                 75.835(2)
_cell_angle_gamma                77.315(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6617(5)
_cell_length_b                   15.7074(8)
_cell_length_c                   18.8918(10)
_cell_measurement_reflns_used    7338
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      22.12
_cell_measurement_theta_min      2.20
_cell_volume                     2542.9(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            79947
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.109
_diffrn_reflns_theta_max         25.109
_diffrn_reflns_theta_min         2.141
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.9224.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9038
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1059P)^2^+5.8102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7166
_reflns_number_total             9038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           sh_231n_0m
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_database_code               7714919
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.936
_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. Restrained distances
 F45-C49 \\sim F45A-C49
 with sigma of 0.02
 C49-F43 \\sim C49-F43A
 with sigma of 0.02
 C49-F44 \\sim C49-F44A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F45) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(F43) \\sim Ueq, Uanis(F44)
\\sim Ueq, Uanis(F43A) \\sim Ueq, Uanis(F45A) \\sim Ueq, Uanis(F44A) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(F43A)=Sof(F45A)=Sof(F44A)=1-FVAR(1)
 Sof(F45)=Sof(F43)=Sof(F44)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C6(H6A,H6B), C11(H11A,H11B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,
 H8B), C12(H12A,H12B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C22(H22), C47(H47), C20(H20), C43(H43), C45(H45)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 193 electrons were 
found in a volume of 935\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C7H8] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39037
_shelx_hkl_checksum              92913
_shelx_fab_checksum              44474
_olex2_submission_special_instructions 'No special instructions were received'