Perfect encapsulation of a guanidinium ion in a helical trinickel(ii) metallocryptand for efficient regulation of the helix inversion rate
Akine, Shigehisa; Miyashita, Masato; Piao, Shunjin; Nabeshima, Tatsuya; Inorg. Chem. Front. 1 (2014) 53–; doi:10.1039/C3QI00067B

data_4350746
_publ_section_title
;
 Perfect encapsulation of a guanidinium ion in a helical trinickel(ii)
 metallocryptand for efficient regulation of the helix inversion rate
;
_journal_issue                   1
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              53
_journal_paper_doi               10.1039/C3QI00067B
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         C124H180N6O26S11
_chemical_formula_sum            'C124 H180 N6 O26 S11'
_chemical_formula_weight         2523.40
_chemical_name_common            C102H108N6O12(Me2SO)11(H2O)3
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   24.1319(10)
_cell_length_b                   24.1319(10)
_cell_length_c                   43.5952(18)
_cell_measurement_reflns_used    39568
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.16
_cell_volume                     21986.3(16)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2009)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_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  'multilayer confocal mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            39568
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9865
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8100
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     1210
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+145.2930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2112
_refine_ls_wR_factor_ref         0.2262
_reflns_number_gt                6674
_reflns_number_total             8570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00067b.txt
_cod_data_source_block           H6L
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4350746