Anion Binding by Dimetallic Nickel(II) and Nickel(III) Complexes of a Face-to-Face Bicyclam: Looking for a Bimacrocyclic Effect.
Boiocchi, Massimo; Fabbrizzi, Luigi; Fusco, Nadia; Invernici, Michele; Licchelli, Maurizio; Poggi, Antonio; Inorganic chemistry 55 (2016) 2946–2959; doi:10.1021/acs.inorgchem.5b02826

data_4347169
_publ_contact_author
;
  Prof Luigi Fabbrizzi
  Dipartimento di Chimica Generale
  University of Pavia
  via Taramelli 12, I-27100 Pavia, ITALY
;
_publ_section_title
;
 Anion Binding by Dimetallic Nickel(II) and Nickel(III) Complexes of a
 Face-to-Face Bicyclam: Looking for a Bimacrocyclic Effect.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2946
_journal_page_last               2959
_journal_paper_doi               10.1021/acs.inorgchem.5b02826
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C32 H62 N8 Ni2, 3(C N O), Cl O4, 2.5 (H2 O) '
_chemical_formula_sum            'C35 H67 Cl N11 Ni2 O9.5'
_chemical_formula_weight         946.87
_chemical_name_common
;
 (mu2-alpha,alpha'-bis((5,7-Dimethyl-1,4,8,11-tetra-azacyclotetradecan-6-yl)
 -o-xylene))-di-nickel(ii) cyanate clathrate dicyanate perchlorate 2.5 hydrate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9118(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5464(5)
_cell_length_b                   25.5845(12)
_cell_length_c                   18.1421(9)
_cell_measurement_reflns_used    8103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     4430.5(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46001
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         9656
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.9751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                6975
_reflns_number_total             9656
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b02826_si_002.cif
_cod_data_source_block           Ni_dicy_NCO
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C35 H67 Cl N11 Ni2 O9.50'
_cod_database_code               4347169