Bimacrocyclic Effect in Anion Recognition by a Copper(II) Bicyclam Complex.
Invernici, Michele; Ciarrocchi, Carlo; Dondi, Daniele; Fabbrizzi, Luigi; Lazzaroni, Simone; Licchelli, Maurizio; Boiocchi, Massimo; Bonizzoni, Marco; ACS omega 3 (2018) 15692–15701; doi:10.1021/acsomega.8b01710

data_4516131
_publ_contact_author
;
  Prof Maurizio Licchelli
  Dipartimento di Chimica Generale
  University of Pavia
  via Taramelli 12, I-27100 Pavia, ITALY
;
_publ_section_title
;
 Bimacrocyclic Effect in Anion Recognition by a Copper(II) Bicyclam
 Complex.
;
_journal_issue                   11
_journal_name_full               'ACS omega'
_journal_page_first              15692
_journal_page_last               15701
_journal_paper_doi               10.1021/acsomega.8b01710
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C32 H62 Cu2 N11, 3 (Cl O4), 0.5 (H2 O)'
_chemical_formula_sum            'C32 H63 Cl3 Cu2 N11 O12.5'
_chemical_formula_weight         1035.36
_chemical_name_common
;
 (mu2-alpha,alpha'-bis((5,7-Dimethyl-1,4,8,11-tetra-azacyclotetradecan-6-yl)
 -o-xylene))-(mu2-azide)-bis(perchlorate)-di-copper(ii) perchlorate hydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6695(14)
_cell_length_b                   18.6531(10)
_cell_length_c                   20.3858(11)
_cell_measurement_reflns_used    6085
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     9380.8(9)
_computing_cell_refinement       'SAINT (Bruker-Axs Inc)'
_computing_data_collection       'SMART (Bruker-Axs Inc)'
_computing_data_reduction        'SAINT (Bruker-Axs Inc)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-Axs Smart-Apex CCD'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85937
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.369
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Krause et al., 2015)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       prism
_exptl_crystal_F_000             4328
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.744
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1798P)^2^+9.1025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6100
_reflns_number_total             8271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b01710_si_002.cif
_cod_data_source_block           Cu2_2_N3_ClO4
_cod_original_formula_sum        'C32 H63 Cl3 Cu2 N11 O12.50'
_cod_database_code               4516131
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              93366
_shelx_hkl_checksum              97217