Reversible structural switch in the nano-cavity of crystalline metallo-macrocycles with smooth ligand exchange by non-coordinating guest stimuli
Ryosuke Miyake; Mitsuhiko Shionoya; Chem.Commun. 48 (2012) 7553–; doi:10.1039/c2cc32857g

data_7108040
_publ_section_title
;
 Reversible structural switch in the nano-cavity of crystalline
 metallo-macrocycles with smooth ligand exchange by non-coordinating guest
 stimuli
;
_journal_name_full               Chem.Commun.
_journal_page_first              7553
_journal_paper_doi               10.1039/c2cc32857g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C48 H130 N36 Ni4 O47'
_chemical_formula_weight         2198.72
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4928(7)
_cell_length_b                   15.4928(7)
_cell_length_c                   19.4045(18)
_cell_measurement_reflns_used    7649
_cell_measurement_temperature    223
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.63
_cell_volume                     4657.6(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17519
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.9147
_exptl_absorpt_correction_T_min  0.8684
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.096(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6713
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0495
_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^)+(0.1043P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1439
_reflns_number_gt                5991
_reflns_number_total             6713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32857g.txt
_cod_data_source_block           i-4_223K
_cod_original_sg_symbol_H-M      'I-4 '
_cod_database_code               7108040