Dynamic covalent chemistry approach toward 18-membered P<sub>4</sub>N<sub>2</sub> macrocycles and their nickel(II) complexes.
Musina, Elvira I.; Wittmann, Tatiana I.; Musin, Lenar; Balueva, Anna S.; Shpagina, Alena S.; Litvinov, Igor A.; Lönnecke, Peter; Hey-Hawkins, Evamarie; Karasik, Andrey A.; Sinyashin, Oleg G.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01317

data_4038870
_publ_section_title
;
 Dynamic covalent chemistry approach toward 18-membered
 P<sub>4</sub>N<sub>2</sub> macrocycles and their nickel(II) complexes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01317
_journal_year                    2020
_chemical_formula_moiety         'C48 H58 N6 O4 P4 [+ solvent]'
_chemical_formula_sum            'C24 H29 N3 O2 P2'
_chemical_formula_weight         453.44
_chemical_melting_point          486
_chemical_name_systematic
;
1,10-Di(4?-methylbenzyl)-3,8,12,17-(RSSR)-tetra(pyridine-2?-yl)-3,8,12,17-
tetraoxo-1,10-diaza?3,8,12,17?tetraphosphacyclooctadecane
;
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                113.230(16)
_cell_angle_beta                 104.32(2)
_cell_angle_gamma                98.18(2)
_cell_formula_units_Z            2
_cell_length_a                   10.11(3)
_cell_length_b                   11.896(16)
_cell_length_c                   12.699(17)
_cell_measurement_reflns_used    637
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.56
_cell_measurement_theta_min      2.86
_cell_volume                     1310(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.1789
_diffrn_reflns_av_unetI/netI     0.2882
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13809
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       formless
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.2882
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0931P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1336
_reflns_number_total             5120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01317_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4038870
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              41665
_shelx_hkl_checksum              11074
_shelx_fab_checksum              26415