Novel ligands from direct benzylic functionalisation of tris(2-pyridylmethyl)amine.
Zardi, Paolo; Piękoś, A, Justyna; Bravin, Carlo; Wurst, Klaus; Droghetti, Federico; Natali, Mirco; Licini, Giulia; Zambon, Alfonso; Zonta, Cristiano; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13831–13836; doi:10.1039/d4dt02022g

data_7716801
_publ_section_title
;
 Novel ligands from direct benzylic functionalisation of
 tris(2-pyridylmethyl)amine.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13831
_journal_page_last               13836
_journal_paper_doi               10.1039/d4dt02022g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C36 H34 N8'
_chemical_formula_weight         578.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.797(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6376(8)
_cell_length_b                   12.1751(8)
_cell_length_c                   19.8852(15)
_cell_measurement_reflns_used    9465
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.3
_cell_volume                     3056.0(4)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex III'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL-XT-2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20404
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.324
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2014/5)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1707 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5047
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0667P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.877
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                4284
_reflns_number_total             5047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02022g2.cif
_cod_data_source_block           2l
_cod_depositor_comments
'Adding full bibliography for 7716800--7716802.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7716801
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              58158
_shelx_hkl_checksum              22257