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_7714913
_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         'C35 H47 N7 Ni O Si, C H2 Cl2'
_chemical_formula_sum            'C36 H49 Cl2 N7 Ni O Si'
_chemical_formula_weight         753.52
_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             2022-10-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                72.352(3)
_cell_angle_beta                 70.181(3)
_cell_angle_gamma                74.277(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4300(8)
_cell_length_b                   13.2816(11)
_cell_length_c                   13.6078(12)
_cell_measurement_reflns_used    6244
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.21
_cell_volume                     1819.1(3)
_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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.1079
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            71977
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.151
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1041 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.9501.
The \l/2 correction factor is Not present.
;
_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    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.854
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0969P)^2^+6.8492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5590
_reflns_number_total             7147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           sh_106n_0m
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_database_code               7714913
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.942
_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 Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C11(H11A,H11B), C6(H6A,H6B), C8(H8A,H8B), C12(H12A,H12B),
 C10(H10A,H10B), C9(H9A,H9B), C7(H7A,H7B), C100(H10C,H10D)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C22(H22), C17(H17), C15(H15)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C31(H31A,H31B,
 H31C), C40(H40A,H40B,H40C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              19685
_shelx_hkl_checksum              31096
_olex2_submission_special_instructions 'No special instructions were received'