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_7718154
_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 H20 Br N3 Ni'
_chemical_formula_sum            'C17 H20 Br N3 Ni'
_chemical_formula_weight         404.98
_chemical_name_systematic        Me
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-12-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-30 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                   9.3768(8)
_cell_length_b                   9.3768(8)
_cell_length_c                   18.877(2)
_cell_measurement_reflns_used    5959
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.43
_cell_volume                     1659.7(3)
_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 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0707
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13329
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.328
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1492 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.5181.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_preparation       Fill
_exptl_crystal_recrystallization_method Fill
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 1071 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3016
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0458P)^2^+1.9843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2598
_reflns_number_total             3016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00135h2.cif
_cod_data_source_block           mo_ed10s_0m
_cod_depositor_comments
'Adding full bibliography for 7718154--7718158.cif.'
_cod_original_cell_volume        1659.8(3)
_cod_database_code               7718154
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.397
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C15(H15A,H15B), C8(H8A,H8B), C10(H10A,H10B)
1.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C4(H4), C11(H11), C6(H6), C12(H12)
1.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              75261
_shelx_hkl_checksum              77731
_olex2_exptl_crystal_mounting_method Fill
_olex2_submission_special_instructions 'No special instructions were received'