Metallo-supramolecular assembly of protic pincer-type complexes: encapsulation of dinitrogen and carbon disulfide into multiproton-responsive diruthenium cage
Toda, Tatsuro; Suzuki, Satoshi; Kuwata, Shigeki; Chemical Communications  (2018) –; doi:10.1039/C8CC08384C

data_7122668
_publ_section_title
;
 Metallo-supramolecular assembly of protic pincer-type complexes:
 encapsulation of dinitrogen and carbon disulfide into
 multiproton-responsive diruthenium cage
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08384C
_journal_year                    2018
_chemical_formula_moiety         'C108 H112 N10 P4 Ru2, 2(H2 O), 1.5(C7 H8)'
_chemical_formula_sum            'C118.5 H128 N10 O2 P4 Ru2'
_chemical_formula_weight         2050.42
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_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_update_record
;
2018-11-23 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            9
_cell_length_a                   47.685(5)
_cell_length_b                   47.685(5)
_cell_length_c                   12.1985(16)
_cell_measurement_reflns_used    12862
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.08
_cell_volume                     24022(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            88358
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.374
_diffrn_reflns_theta_min         3.081
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9657.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.36
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     533
_refine_ls_number_reflns         11981
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1209P)^2^+57.3279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9852
_reflns_number_total             11981
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8cc08384c2.cif
_cod_data_source_block           compound3-2H2O-C7H8
_cod_original_cell_volume        24021(5)
_cod_database_code               7122668
_shelx_res_checksum              82305
_shelx_hkl_checksum              66612
_shelx_fab_checksum              57157