C-C and C-O bond formation reactivity of nickel complexes supported by the pyridinophane <sup>Me</sup>N3C ligand.
Leung, Joshua Ji-Nung; Bae, Dae Young; Moshood, Yusuff; Mirica, Liviu M.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5286–5292; doi:10.1039/d5dt00135h

data_7718155
_publ_section_title
;
 C-C and C-O bond formation reactivity of nickel complexes supported by
 the pyridinophane <sup>Me</sup>N3C ligand.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5286
_journal_page_last               5292
_journal_paper_doi               10.1039/d5dt00135h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C17 H21 Cl2 N3 Ni, C2 H3 N'
_chemical_formula_sum            'C19 H24 Cl2 N4 Ni'
_chemical_formula_weight         438.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-23 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6090(4)
_cell_length_b                   8.7670(2)
_cell_length_c                   14.6494(3)
_cell_measurement_reflns_used    26085
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.61
_cell_volume                     2004.68(8)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33927
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         2.323
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.8396.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.838
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.368
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2326 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0188
_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^)+(0.0233P)^2^+0.6494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0475
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4939
_reflns_number_total             4996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00135h2.cif
_cod_data_source_block           mo_ed45x
_cod_depositor_comments
'Adding full bibliography for 7718154--7718158.cif.'
_cod_database_code               7718155
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.422
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C8(H8A,H8B), C15(H15A,H15B)
1.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C11(H11), C10(H10), C3(H3)
1.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              11680
_shelx_hkl_checksum              28230
_olex2_submission_special_instructions 'No special instructions were received'