Two-step modulation of ion recognition using a bis(saloph)-macrocyclic host having a 24-crown-8-like cavity
Sakata, Yoko; Kobayashi, Seiya; Akine, Shigehisa; Chem. Commun.  (2017) –; doi:10.1039/C7CC02641B

data_7120150
_publ_section_title
;
 Two-step modulation of ion recognition using a bis(saloph)-macrocyclic
 host having a 24-crown-8-like cavity
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02641B
_journal_year                    2017
_chemical_formula_moiety         C46H34Cl6N4Ni2O8
_chemical_formula_sum            'C46 H34 Cl6 N4 Ni2 O8'
_chemical_formula_weight         1100.89
_chemical_name_common            '[LNi2]_2CHCl3'
_chemical_name_systematic        LNi2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-31 deposited with the CCDC.
2017-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.672(4)
_cell_length_b                   7.4623(10)
_cell_length_c                   21.658(3)
_cell_measurement_reflns_used    13621
_cell_measurement_temperature    93
_cell_measurement_theta_max      24.994
_cell_measurement_theta_min      2.423
_cell_volume                     4310.7(11)
_computing_cell_refinement       'APEX2 v2014.9 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service V4.2.2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXD (Sheldrick, 2000)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer confocal mirror'
_diffrn_radiation_source         'micro focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1881
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       column
_exptl_crystal_F_000             2240
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3/MeOH'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2001
_refine_ls_number_restraints     307
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0878
_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^)+(0.0299P)^2^+37.1099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1157
_reflns_number_total             2001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02641b2.cif
_cod_data_source_block           koba001
_cod_original_cell_volume        4310.8(11)
_cod_database_code               7120150
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              66592
_shelx_hkl_checksum              3811