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_7714909
_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         'C51 H53 N7 Ni S, 2(C7 H8)'
_chemical_formula_sum            'C65 H69 N7 Ni S'
_chemical_formula_weight         1039.04
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-12
_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                90
_cell_angle_beta                 103.02(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.78(5)
_cell_length_b                   17.42(5)
_cell_length_c                   20.19(6)
_cell_measurement_reflns_used    7964
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      23.38
_cell_measurement_theta_min      2.37
_cell_volume                     5407(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9661
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.182
_diffrn_reflns_theta_max         25.182
_diffrn_reflns_theta_min         1.891
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1097 before and 0.0649 after correction.
 
For component 2:
 wR2(int) was 0.1080 before and 0.0689 after correction.
 The Ratio of minimum to maximum transmission is 0.93.

Final HKLF 4 output contains 152352 reflections, Rint = 0.1968
 (25941 with I > 3sig(I), Rint = 0.0575)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         9661
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.1073
_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^)+45.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7424
_reflns_number_total             9661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03746k2.cif
_cod_data_source_block           test4_a
_cod_depositor_comments
'Adding full bibliography for 7714908--7714920.cif.'
_cod_original_cell_volume        5408(28)
_cod_database_code               7714909
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5662(19)
 0.4338(19)
2. 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
3. Restrained distances
 C100-C105
 1.39 with sigma of 0.01
 C100-C101 \\sim C102-C103 \\sim C104-C105
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C106) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C104) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C101) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C28A) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: C28(0.67) H28A(0.67) H28B(0.67) H28C(0.67) C26(0.67) H26A(0.67)
 H26B(0.67) H26C(0.67) C27(0.67) H27A(0.67) H27B(0.67) H27C(0.67) C26A(0.33)
 H26D(0.33) H26E(0.33) H26F(0.33) C28A(0.33) H28D(0.33) H28E(0.33) H28F(0.33)
 C27A(0.33) H27D(0.33) H27E(0.33) H27F(0.33)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C7(H7A,H7B), C9(H9A,H9B), C6(H6A,H6B), C5(H5A,H5B), C10(H10A,
 H10B), C8(H8A,H8B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C49(H49), C48(H48), C52(H52), C58(H58), C50(H50), C46(H46),
 C22(H22), C20(H20), C15(H15), C54(H54), C17(H17), C55(H55), C42(H42), C57(H57),
  C44(H44), C56(H56), C201(H201), C45(H45), C204(H204), C43(H43), C203(H203),
 C205(H205), C202(H202), C103(H103), C102(H102), C105(H105), C101(H101),
 C104(H104)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C206(H20A,H20B,
 H20C), C106(H10C,H10D,H10E), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C26A(H26D,H26E,H26F), C28A(H28D,H28E,H28F), C27A(H27D,
 H27E,H27F)
;
_shelx_res_checksum              11415
_shelx_hkl_checksum              23315
_olex2_submission_special_instructions 'No special instructions were received'