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_4350747
_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         C137H180Cl10N6Ni3O16S3
_chemical_formula_sum            'C137 H180 Cl10 N6 Ni3 O16 S3'
_chemical_formula_weight         2793.68
_chemical_name_common            '[LNi3]_3DMSO_H2O_5DCM_4cyclohex'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.974(2)
_cell_angle_beta                 83.133(2)
_cell_angle_gamma                82.959(2)
_cell_formula_units_Z            2
_cell_length_a                   17.1680(6)
_cell_length_b                   19.0600(7)
_cell_length_c                   25.3558(9)
_cell_measurement_reflns_used    52060
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.21
_cell_volume                     7608.9(5)
_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    'DIRDIF99 (Beurskens et al., 1999)'
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52060
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.8561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.333
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2492
_refine_ls_number_reflns         26699
_refine_ls_number_restraints     1156
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0987
_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^)+(0.0213P)^2^+37.6268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2444
_reflns_number_gt                15452
_reflns_number_total             26699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00067b.txt
_cod_data_source_block           LNi3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4350747