Single-crystal X-ray diffraction study, NMR and electrochemical analysis of a copper(i) 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis-[(6-methyl-2,2′-bipyridyl-6-yl)methoxy]calix[4]arene complex: an original M4L2 “hand-to-hand” system
Regnouf-de-Vains, J.-B.; Malaman, B.; Bouguet-Bonnet, S.; Poinsignon, Sophie; Leclerc, Sébastien; Beley, M.; New Journal of Chemistry 43 (2019) 13282–; doi:10.1039/C9NJ01152H

data_7058658
_publ_section_title
;
 Single-crystal X-ray diffraction study, NMR and electrochemical analysis
 of a copper(i)
 5,11,17,23-tetra-tert-butyl-25,26,27,28-tetrakis-[(6-methyl-2,2&#x2032;-bipyridyl-6-yl)methoxy]calix[4]arene
 complex: an original M4L2 &#x201C;hand-to-hand&#x201D; system
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13282
_journal_paper_doi               10.1039/C9NJ01152H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C184 H192 Cu4 N16 O8 P4 F24'
_chemical_formula_sum            'C184 H192 Cu4 F24 N16 O8 P4'
_chemical_formula_weight         3589.57
_chemical_name_systematic
'biscopper(I) 5,11,17,23-Tetra-tert-butyl-25,26,27,28-tetrakis-[(6-methyl-2,2'-bipyridyl-6-\ yl)methoxy]calix[4]arene, tetra(hexafluorophosphate)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-11-06 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                109.518(3)
_cell_angle_beta                 101.629(3)
_cell_angle_gamma                97.800(3)
_cell_formula_units_Z            2
_cell_length_a                   19.225(2)
_cell_length_b                   22.570(3)
_cell_length_c                   27.113(3)
_cell_measurement_reflns_used    2432
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      2.22
_cell_volume                     10595(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER APEX II QUAZAR CCD'
_diffrn_measurement_method       'f\ and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         ImuS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42887
_diffrn_reflns_theta_full        14.85
_diffrn_reflns_theta_max         14.85
_diffrn_reflns_theta_min         1.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.50
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepided
_exptl_crystal_F_000             3716
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/toluene'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.502
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         8293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.502
_refine_ls_R_factor_all          0.2090
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          23.352
_refine_ls_shift/su_mean         0.461
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3788
_refine_ls_wR_factor_ref         0.4061
_reflns_number_gt                5182
_reflns_number_total             8293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj01152h2.cif
_cod_data_source_block           JBI143-centre
_cod_depositor_comments          'Adding full bibliography for 7058658.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C184 H192 Cu4 N16 O8 P4 F24'
_cod_database_code               7058658